JP3045207B2 - Production method of plate-like iron oxide particles - Google Patents

Production method of plate-like iron oxide particles

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Publication number
JP3045207B2
JP3045207B2 JP4224764A JP22476492A JP3045207B2 JP 3045207 B2 JP3045207 B2 JP 3045207B2 JP 4224764 A JP4224764 A JP 4224764A JP 22476492 A JP22476492 A JP 22476492A JP 3045207 B2 JP3045207 B2 JP 3045207B2
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Japan
Prior art keywords
plate
particles
hematite
thickness
iron oxide
Prior art date
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JP4224764A
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Japanese (ja)
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JPH0656429A (en
Inventor
勉 片元
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Toda Kogyo Corp
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Toda Kogyo Corp
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Description

【発明の詳細な説明】DETAILED DESCRIPTION OF THE INVENTION

【0001】[0001]

【産業上の利用分野】本発明は、粒度が均斉であって配
向性が優れており、しかも粒子の厚みが制御された板状
酸化鉄粒子粉末の製造法に関するものである。本発明に
係る板状酸化鉄粒子粉末の主な用途は、塗料用、印刷イ
ンキ用、化粧品用、樹脂成形物用等の着色顔料、電磁波
吸収用、シールド用、制振用、防音用、磁気トナー用、
磁気記録用等の材料である。
BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing plate-like iron oxide particles having a uniform particle size, excellent orientation and a controlled particle thickness. The main uses of the plate-like iron oxide particles according to the present invention include coatings, printing inks, cosmetics, coloring pigments for resin moldings, electromagnetic wave absorption, shielding, vibration suppression, soundproofing, magnetic For toner,
It is a material for magnetic recording and the like.

【0002】[0002]

【従来の技術】酸化鉄顔料としては、赤〜赤茶系を呈す
るヘマタイト(α−Fe23 )粒子粉末、黒色系を呈
するマグネタイト(FeO x ・Fe23 0<x≦
1)粒子粉末、茶褐色系を呈するマグヘマイト(γ−F
23 )粒子粉末が知られており、これら粒子粉末は
いずれもビヒクル中に混合分散して塗料、印刷インキ、
化粧品等を製造したり、樹脂中に混練分散した後成形し
て樹脂成形物を製造したりする際の着色顔料として広く
使用されている。また、酸化鉄顔料のうち板状形態を呈
した酸化鉄顔料は、その形態に起因して板状粒子が配向
しやすい為、被覆性に優れているという特性を生かし
て、防錆顔料として使用されたり、その有する金属光沢
を生かして自動車等の上塗塗料用着色顔料としても使用
されている。
2. Description of the Related Art As iron oxide pigments, hematite (α-Fe 2 O 3 ) particles powder exhibiting red to reddish brown, and magnetite ( FeO x .Fe 2 O 3 0 <x ≦
1) Particle powder, brown-colored maghemite (γ-F
e 2 O 3 ) particle powders are known, and all of these particle powders are mixed and dispersed in a vehicle to prepare paints, printing inks,
It is widely used as a coloring pigment for producing cosmetics and the like, or kneading and dispersing in a resin, followed by molding to produce a resin molded product. In addition, among iron oxide pigments, iron oxide pigments having a plate-like shape are used as rust preventive pigments by taking advantage of the property of being excellent in coverage because plate-like particles are easily oriented due to the shape. It is also used as a coloring pigment for top coats of automobiles and the like by utilizing its metallic luster.

【0003】更に、マグネタイト粒子やマグヘマイト粒
子は、上述した通り、着色顔料として使用されていると
ともにその有する磁気特性を生かして、電磁波吸収用、
シールド用、制振用、防音用、磁性トナー用、磁気記録
用材料として各種分野で使用されているが、特に板状形
態を呈したマグネタイト粒子やマグヘマイト粒子は、そ
の形態に起因する特性を有効に活用することが期待され
ている。
[0003] Further, as described above, magnetite particles and maghemite particles are used as color pigments and take advantage of their magnetic properties to absorb electromagnetic waves.
It is used in various fields as a material for shielding, vibration damping, soundproofing, magnetic toner, and magnetic recording.Especially, plate-like magnetite particles and maghemite particles are effective in their properties. It is expected to be used for

【0004】この事実は、例えば、特公昭63−418
53号公報の「薄片形磁性酸化鉄粒子を一つもしくはそ
れ以上の磁化性層を含む磁気テープ、カードまたは円板
のごとき磁気記録支持体に用いる可能性が開かれ
る。」、「マグネタイトまたはマグヘマイトの結晶構造
を有する六角薄片形酸化鉄に対する他の用途がある。‥
‥被覆材料中に個々の粒子の極めて顕著な平行配向が生
ずる。従って、‥‥著しく高い充填密度を得ることが可
能であり、その結果例えば腐食防止効果が増大し、電磁
気干渉場に対する遮蔽が効果的となり、そして導電性が
高くなる。」なる記載及び特開昭61−138959号
公報の「一成分トナーの磁性の成分として小板状または
鱗片状の磁化しうる粒子を用いるとき、トナーの色が決
定されるのは磁性成分それ自体の本来の色によることは
僅かであり主として添加された強い色の着色剤によるこ
とが見出された。」、「これら粒子は次に簡単に攪拌す
るだけで何ら特別の分級エネルギーを消費することなし
に、結合剤または結合剤溶液中における良好な分散状態
へと直ちに転換することができる。」なる記載の通りで
ある。
This fact is described, for example, in JP-B-63-418.
No. 53, "Opening the possibility of using flaky magnetic iron oxide particles for magnetic recording supports such as magnetic tapes, cards or discs containing one or more magnetic layers", "Magnetite or maghemite. There is another application for hexagonal flake iron oxide having the following crystal structure.
極 め て A very pronounced parallel orientation of the individual particles occurs in the coating material. Therefore, it is possible to achieve a significantly higher packing density, which results in, for example, an increased corrosion protection effect, more effective shielding against electromagnetic interference fields and higher conductivity. And Japanese Patent Application Laid-Open No. 61-138959, "When platelet-like or scale-like magnetizable particles are used as the magnetic component of a one-component toner, the color of the toner is determined by the magnetic component itself. Was found to be slightly and mainly due to the strong colorant added. "," These particles then consume any special classification energy with a simple stirring. Without a rapid conversion to a good dispersion in the binder or binder solution. "

【0005】上述した通り、板状形態の酸化鉄粒子粉末
は各種分野で使用されているが、前述いずれの分野にお
いても色や磁性等の本来の機能を十分発揮することはも
ちろん被覆性、遮蔽性等の形態上の諸特性を十分発揮す
る為にはビヒクルへの混合分散、樹脂への混練分散に際
して分散性と配向性が優れているとともに樹脂の種類や
溶剤の種類等に応じて樹脂になじみやすい好適な厚みに
自由に制御できることが強く要求されている。
As described above, plate-like iron oxide particles are used in various fields. In any of the above-mentioned fields, the iron oxide particle powders can sufficiently exhibit their original functions such as color and magnetism, as well as covering properties and shielding properties. In order to sufficiently exhibit various morphological properties such as dispersibility, it is excellent in dispersibility and orientation when mixing and dispersing in a vehicle, kneading and dispersing in a resin, and at the same time, depending on the type of resin and the type of solvent, There is a strong demand that the thickness can be freely controlled to a suitable thickness that is easy to conform to.

【0006】板状酸化鉄粒子粉末の分散性を改良する為
には、粒度ができるだけ均斉であることが望ましく、配
向性の向上の為には、板状酸化鉄粒子粉末の集合状態が
面内方向で粒子相互が重なり合って連続的に配列してい
ることが好ましい。
[0006] In order to improve the dispersibility of the plate-like iron oxide particles, it is desirable that the particle size be as uniform as possible. It is preferable that the particles overlap in the direction and are continuously arranged.

【0007】従来、板状ヘマタイト粒子粉末の製造法と
しては、含水酸化第二鉄粒子又は第二鉄塩を含むアル
カリ性懸濁液を水熱処理する方法(特公昭43−124
35号公報、特公昭45−54号公報、特公昭48−2
9718号公報、特公昭49−44878号公報、特公
昭63−41853号公報)含水酸化第二鉄粒子又は
第二鉄塩を含むアルカリ懸濁液中に、生成する板状ヘマ
タイト粒子の粒度を均斉にする為種晶として板状ヘマタ
イト粒子を添加した後水熱処理する方法(特公昭55−
16978号公報、特開昭50−34000号公報、特
開昭61−174120号公報)等が知られている。
Conventionally, as a method of producing plate-like hematite particles, a method of hydrothermally treating an alkaline suspension containing ferric hydroxide particles or a ferric salt (Japanese Patent Publication No. 43-124).
No. 35, JP-B-45-54, JP-B-48-2
9718, JP-B-49-44878, JP-B-63-41853) The size of plate-like hematite particles formed in an alkaline suspension containing ferric hydroxide particles or a ferric salt is uniformized. Method of adding plate-like hematite particles as seed crystals and subjecting them to hydrothermal treatment
16978, JP-A-50-34000, JP-A-61-174120) and the like.

【0008】板状マグネタイト粒子は、水溶液中から生
成した板状ヘマタイト粒子を還元性雰囲気中300〜4
50℃の温度範囲で加熱還元することにより、板状マグ
ヘマイト粒子は、板状マグネタイト粒子を更に200〜
400℃の温度範囲で酸化することにより得られる。得
られた板状マグネタイト粒子や板状マグヘマイト粒子は
板状ヘマタイト粒子のサイズや形態、そして集合状態を
保持継承している。
The plate-like magnetite particles are formed by reducing plate-like hematite particles generated from an aqueous solution in a reducing atmosphere to 300 to 4 times.
By heating and reducing in a temperature range of 50 ° C., the plate-like maghemite particles further reduce the plate-like magnetite particles by 200 to
It is obtained by oxidizing in a temperature range of 400 ° C. The obtained plate-like magnetite particles and plate-like maghemite particles retain and inherit the size, shape, and aggregation state of the plate-like hematite particles.

【0009】[0009]

【発明が解決しようとする課題】粒度が均斉で配向性が
優れており、粒子の厚みが制御された板状酸化鉄粒子粉
末は現在最も要求されているところであるが、前出公知
の方法によって得られた板状酸化鉄粒子粉末はこれら諸
特性を十分満たすものではない。
Plate-like iron oxide particles having a uniform particle size and excellent orientation and having a controlled particle thickness are the most demanded at present. The obtained plate-like iron oxide particles do not sufficiently satisfy these properties.

【0010】即ち、前出の公知方法は後出比較例1の
電子顕微鏡写真に示される通り、前出の公知方法に比
べ粒度は比較的均斉であるが、粒子の厚みが厚いことに
よって個々の板状粒子の向きが一様ではなく、しかも、
個々の粒子が独立して存在している為、配向性が十分と
はいえない。
That is, as shown in the electron micrograph of Comparative Example 1 described above, the particle size is relatively uniform in the above-mentioned known method as compared with the above-mentioned known method. The direction of the plate-like particles is not uniform, and
Since the individual particles exist independently, the orientation is not sufficient.

【0011】前出の公知方法は、後出比較例2の電子
顕微鏡写真に示される通り、個々の板状粒子がほぼ一定
方向を向いているが、種晶として添加した板状ヘマタイ
ト粒子の反応性が小さい為、該種晶の成長反応が一様に
生起せず、かえって粒度が不均斉となりやすいものであ
る。
According to the above-mentioned known method, as shown in the electron micrograph of Comparative Example 2 below, the individual plate-like particles are oriented in a substantially constant direction, but the reaction of the plate-like hematite particles added as seed crystals. Due to the low property, the seed crystal growth reaction does not occur uniformly, and the particle size tends to be uneven.

【0012】また、前出及びの方法による場合に
は、水熱処理中の反応温度やアルカリ濃度により、生成
する板状ヘマタイト粒子の厚みを制御することができる
ことが知られているが、厚みが厚い板状ヘマタイト粒子
が生成しやすく、一般に配向性がよいといわれている厚
みが0.5μm程度未満の板状ヘマタイト粒子は生成し
がたく、しかも粒子の厚みの変化率が小さいものである
から、0.5μm程度未満の範囲内での粒子の厚みの制
御は困難である。
In the above-mentioned methods, it is known that the thickness of the plate-like hematite particles to be produced can be controlled by the reaction temperature or the alkali concentration during the hydrothermal treatment. Plate-like hematite particles are easily generated, and plate-like hematite particles having a thickness of less than about 0.5 μm, which is generally said to have good orientation, are difficult to generate, and since the rate of change in particle thickness is small, It is difficult to control the thickness of the particles within a range of less than about 0.5 μm.

【0013】そこで、本発明は、粒度が均斉であって配
向性が優れており、しかも粒子の厚みが制御された板状
酸化鉄粒子粉末を得ることを技術的課題とする。
Accordingly, an object of the present invention is to provide a plate-like iron oxide particle powder having a uniform particle size, excellent orientation, and a controlled particle thickness.

【0014】[0014]

【問題点を解決するための手段】前記技術的課題は、次
の通りの本発明によって達成できる。即ち、本発明は、
含水酸化第二鉄粒子又は第二鉄塩を含むpH11以上の
アルカリ性懸濁液を水熱処理することによって板状ヘマ
タイト粒子粉末を生成させる方法において、前記アルカ
リ性懸濁液中にあらかじめ種晶として針状含水酸化第二
鉄粒子を加熱処理して得られる針状ヘマタイト粒子を添
すると共に、pHを11以上とし、且つ、アルカリ濃
度を0.3〜0.7Nの範囲とし、次いで150〜33
0℃の温度範囲で水熱処理することにより厚みが0.5
μm以下の板状ヘマタイト粒子を生成させるか、必要に
より、該板状ヘマタイト粒子を加熱還元して板状マグネ
タイト粒子とするか、又は、更に酸化して板状マグヘマ
イト粒子とすることからなる板状酸化鉄粒子粉末の製造
法である。
The above technical problems can be achieved by the present invention as described below. That is, the present invention
In a method of producing plate-like hematite particle powder by hydrothermally treating an alkaline suspension having a pH of 11 or more containing hydrous ferric oxide particles or a ferric salt, a needle-like form is previously prepared as a seed crystal in the alkaline suspension. Needle-like hematite particles obtained by heat-treating the hydrous ferric oxide particles are added , the pH is adjusted to 11 or more, and
Degree in the range 0.3-0.7N , then 150-33
Hydrothermal treatment in a temperature range of 0 ° C has a thickness of 0.5
μm or less plate-like hematite particles, if necessary, the plate-like hematite particles are reduced by heating to plate-like magnetite particles, or further oxidized to plate-like maghemite particles This is a method for producing iron oxide particles.

【0015】次に、本発明実施にあたっての諸条件につ
いて述べる。
Next, various conditions for implementing the present invention will be described.

【0016】本発明における含水酸化第二鉄粒子として
は、周知の各種反応により得られた針状、紡錘状等のい
ずれの粒子形態のものでもよく、含水酸化第二鉄を含む
生成反応母液、該反応母液を水洗、濾過して得られた湿
ケーキ及び該湿ケーキの乾燥物を使用することができ
る。
The hydrous ferric oxide particles in the present invention may be in the form of any of needles, spindles, and the like obtained by various known reactions. A wet cake obtained by washing and filtering the reaction mother liquor and a dried product of the wet cake can be used.

【0017】本発明における第二鉄塩としては、硝酸第
二鉄、塩化第二鉄、硫酸第二鉄等を使用することができ
る。
As the ferric salt in the present invention, ferric nitrate, ferric chloride, ferric sulfate and the like can be used.

【0018】本発明におけるアルカリ性懸濁液のpHは
11以上である。11未満である場合には、板状ヘマタ
イト粒子中に針状含水酸化第二鉄粒子又は水酸化第二鉄
が混在する。また、反応時間が長時間となり工業的では
ない。
The pH of the alkaline suspension of the present invention is 11 or more. If it is less than 11, acicular ferric hydroxide oxide particles or ferric hydroxide are mixed in the plate-like hematite particles. In addition, the reaction time is long, which is not industrial.

【0019】本発明における水熱処理は、オートクレー
ブ装置を用い、通常150〜330℃の温度範囲で行
う。一般にアルカリ濃度が濃くなる程、板状ヘマタイト
粒子の生成する反応温度は低くなる傾向にある。150
℃未満の場合には、含水酸化第二鉄や針状ヘマタイト粒
子がそのまま存在し、板状ヘマタイト粒子が生成しな
い。330℃を越える場合にも板状ヘマタイト粒子の生
成は可能であるが、装置上の安全性等を考慮した場合、
温度の上限は330℃である。
The hydrothermal treatment in the present invention is carried out usually in a temperature range of 150 to 330 ° C. using an autoclave apparatus. Generally, as the alkali concentration becomes higher, the reaction temperature at which plate-like hematite particles are formed tends to be lower. 150
When the temperature is lower than ° C, hydrous ferric oxide and acicular hematite particles are present as they are, and plate-like hematite particles are not generated. Although it is possible to generate plate-like hematite particles even when the temperature exceeds 330 ° C., considering safety on the device,
The upper limit of the temperature is 330 ° C.

【0020】本発明における種晶として添加する針状ヘ
マタイト粒子は、針状含水酸化第二鉄粒子を加熱処理す
ることにより得ることができる。加熱処理温度は260
〜700℃が好ましい。260℃未満である場合には、
針状含水酸化第二鉄粒子の脱水反応が不十分で、種晶と
しての効果が少なく、本発明の目的とする板状ヘマタイ
ト粒子を得ることができない。700℃を越える場合に
は、針状粒子及び粒子相互間の焼結が起こり、本発明の
目的とする配向性のよい板状ヘマタイト粒子を生成させ
ることが困難である。
The acicular hematite particles to be added as seed crystals in the present invention can be obtained by heat-treating acicular hydrous ferric oxide particles. Heat treatment temperature is 260
~ 700 ° C is preferred. If it is less than 260 ° C,
The dehydration reaction of the needle-like hydrous ferric oxide particles is insufficient, the effect as a seed crystal is small, and the plate-like hematite particles intended in the present invention cannot be obtained. When the temperature exceeds 700 ° C., sintering between the acicular particles and the particles occurs, and it is difficult to produce the plate-like hematite particles having good orientation, which is the object of the present invention.

【0021】針状ヘマタイト粒子は、Fe以外のTi、
Ni、Co、Zr等を含有していてもよく、これら元素
を含有していることによって、粒子の厚みがより薄くな
って配向性に優れた板状ヘマタイト粒子が生成しやすく
なり、より効果的に本発明の目的とする板状ヘマタイト
粒子粉を得ることができる。
The acicular hematite particles include Ti other than Fe,
Ni, Co, Zr or the like may be contained, and by containing these elements, plate-like hematite particles having a thinner particle thickness and excellent orientation can be easily generated, which is more effective. Thus, a plate-like hematite particle powder intended for the present invention can be obtained.

【0022】Tiは、0.1〜20mol%、Ni、C
o及びZrは0.1〜10mol%を針状ヘマタイト粒
子中に含有させることができ、本発明の目的とする板状
ヘマタイト粒子粉末を効果的に得る為にはTi含有針状
ヘマタイト粒子を種晶として用いることが好ましい。
Ti is 0.1 to 20 mol%, Ni, C
As for o and Zr, 0.1 to 10 mol% can be contained in the acicular hematite particles, and in order to effectively obtain the plate-like hematite particle powder intended for the present invention, the Ti-containing acicular hematite particles are seeded. It is preferably used as a crystal.

【0023】針状ヘマタイト粒子の添加量は、第二鉄1
molに対し0.005〜20mol%である。0.0
05mol%未満の場合には、種晶としての効果が不十
分であり、本発明の目的とする配向性のよい板状酸化鉄
粒子が得られない。20mol%を越える場合には、生
成するヘマタイト粒子の粒子形状が針状になり、粒子の
配向性が悪い。
The amount of the acicular hematite particles added is
It is 0.005 to 20 mol% based on mol. 0.0
When the content is less than 05 mol%, the effect as a seed crystal is insufficient, and the plate-like iron oxide particles having good orientation intended in the present invention cannot be obtained. If it exceeds 20 mol%, the hematite particles to be formed become acicular in shape, and the orientation of the particles is poor.

【0024】本発明における板状マグネタイト粒子とす
る際の加熱還元温度は300〜450℃である。300
℃未満の場合には、還元反応の進行が著しく遅く、長時
間を要する。450℃を越える場合には、粒子相互間で
焼結が生起する。
The heat reduction temperature of the plate-like magnetite particles in the present invention is 300 to 450 ° C. 300
If the temperature is lower than 0 ° C, the progress of the reduction reaction is extremely slow, and it takes a long time. If it exceeds 450 ° C., sintering occurs between the particles.

【0025】本発明における板状マグヘマイト粒子とす
る際の酸化温度は、200〜400℃である。200℃
未満の場合には、酸化反応の進行が著しく遅く、長時間
を要する。400℃を越える場合には、急激な酸化反応
が起き、ヘマタイトへの変態が生起し、ヘマタイト粒子
が混在してくる。
The oxidation temperature for forming plate-like maghemite particles in the present invention is 200 to 400 ° C. 200 ° C
If it is less than 1, the progress of the oxidation reaction is extremely slow, and it takes a long time. When the temperature exceeds 400 ° C., a rapid oxidation reaction occurs, transformation to hematite occurs, and hematite particles are mixed.

【0026】[0026]

【作用】先ず、本発明において最も重要な点は、含水酸
化第二鉄粒子又は第二鉄塩を含むpH11以上のアルカ
リ性懸濁液を水熱処理することによって板状ヘマタイト
粒子粉末を生成させる方法において、前記アルカリ性懸
濁液中にあらかじめ種晶として針状含水酸化第二鉄粒子
を加熱処理して得られる針状ヘマタイト粒子を添加する
と共に、pHを11以上とし、且つ、アルカリ濃度を
0.3〜0.7Nの範囲とし、次いで150〜330℃
の温度範囲で水熱処理した場合には、粒度が均斉であっ
て配向性が優れており、しかも粒子の厚みを制御するこ
とができるという事実である。
First, the most important point in the present invention is that a plate-like hematite particle powder is produced by hydrothermally treating an alkaline suspension containing ferric hydroxide particles or a ferric salt having a pH of 11 or more. The needle-like hematite particles obtained by heat-treating the needle-like hydrous ferric oxide particles as seed crystals in advance in the alkaline suspension are added .
At the same time, the pH is adjusted to 11 or more, and the alkali concentration is adjusted to
0.3-0.7N range, then 150-330 ° C
This is a fact that when the hydrothermal treatment is performed in the above temperature range , the particle size is uniform, the orientation is excellent, and the thickness of the particles can be controlled.

【0027】本発明者は、粒度が均斉な板状ヘマタイト
粒子が得られる理由について、後出実施例に示す通り、
板状ヘマタイト粒子の生成反応が短時間裡に終了するこ
とから、針状含水酸化第二鉄粒子を加熱処理して得られ
る針状ヘマタイト粒子の反応性が大きいことにより針状
ヘマタイト粒子を種晶とする成長反応が一斉に開始する
ためであろうと考えている。
The present inventor has described the reason why plate-like hematite particles having a uniform particle size can be obtained, as will be described in Examples below.
Since the reaction of forming plate-like hematite particles is completed in a short time, the needle-like hematite particles obtained by heating the needle-like hydrous ferric oxide particles have high reactivity, so that the needle-like hematite particles can be seeded. It is thought that this is because the growth reaction starts at the same time.

【0028】また、配向性が優れている理由について、
本発明者は、粒子の厚みが0.5μm程度以下と適度に
薄いこと、面内方向で粒子相互が重なり合って連続的に
配列していること及び後出実施例の電子顕微鏡写真に示
す通り、生成板状ヘマタイト粒子の板面のほぼ中央付近
に孔があるものが多量に存在しているという粒子の構造
的特徴によるものと考えている。この粒子中央付近の孔
は、種晶として用いた針状ヘマタイト粒子のうち、反応
性の良い針状ヘマタイト粒子が溶解析出反応したために
生成されたものと考えている。
The reason why the orientation is excellent is as follows.
The present inventors have found that the thickness of the particles is appropriately thin as about 0.5 μm or less, that the particles are continuously arranged in an in-plane direction overlapping each other, and as shown in the electron micrographs of Examples described later, This is considered to be due to the structural characteristics of the resulting plate-like hematite particles, which have a large amount of holes near the center of the plate surface. It is considered that the pores near the center of the particles were generated due to the dissolution reaction of acicular hematite particles having good reactivity among the acicular hematite particles used as seed crystals.

【0029】本発明においては、反応温度、アルカリ濃
度及び針状ヘマタイト粒子の厚みにより生成する板状ヘ
マタイト粒子の厚みを0.5μm以下、殊に0.05〜
0.5μmの範囲で自由に制御することができる。
In the present invention, the thickness of the plate-like hematite particles formed depending on the reaction temperature, the alkali concentration and the thickness of the acicular hematite particles is 0.5 μm or less, especially 0.05 to 0.05 μm.
It can be controlled freely within the range of 0.5 μm.

【0030】今、本発明者が行った数多くの実験例から
その一部を抽出して説明すれば、以下の通りである。
Now, a description will be given of a part of a number of experimental examples conducted by the present inventor as described below.

【0031】図1乃至図3の各図は、生成した板状ヘマ
タイト粒子粉末の厚みと反応温度、アルカリ濃度、針状
ヘマタイト粒子の厚みのそれぞれとの関係を示したもの
である。図1中、曲線A、B及びCはそれぞれ、後出実
施例4、比較例1(前出の公知方法のうちの特公昭4
3−12435号公報に該当する。)及び比較例2(前
出の公知方法のうち特公昭55−16978号公報に
該当する。)と同様の条件下で反応温度をふらした場合
である。図1に示される通り、本発明においては、粒子
の厚みを0.5μm以下という薄い範囲で効果的に制御
することができる。
FIGS. 1 to 3 show the relationship between the thickness of the produced plate-like hematite particles, the reaction temperature, the alkali concentration, and the thickness of the acicular hematite particles. In FIG. 1, curves A, B and C are respectively shown in Example 4 and Comparative Example 1 described later (Japanese Patent Publication No.
This corresponds to JP-A-3-12435. ) And Comparative Example 2 (corresponding to Japanese Patent Publication No. 55-16978 among the known methods described above) in which the reaction temperature was varied under the same conditions. As shown in FIG. 1, in the present invention, the thickness of the particles can be effectively controlled in a thin range of 0.5 μm or less.

【0032】図2は、後出実施例4と同様の条件下でア
ルカリ濃度をふらした場合であり、同図に示される通
り、本発明においては粒子の厚みを配向性が良いといわ
れている0.5μm程度未満で、より効果的に制御する
ことができる。図3は後出実施例4と同様の条件下で種
晶である針状ヘマタイト粒子の厚みを種々変化させた場
合であり、同図に示される通り本発明においては、粒子
の厚みを配向性が良いといわれている0.5μm程度以
下でより効果的に制御することができる。
FIG. 2 shows a case where the alkali concentration is varied under the same conditions as in Example 4 described later. As shown in FIG. 2, in the present invention, the thickness of the particles is said to have good orientation. When the thickness is less than about 0.5 μm, more effective control can be achieved. FIG. 3 shows the case where the thickness of the acicular hematite particles as seed crystals was variously changed under the same conditions as in Example 4 described later, and as shown in FIG. Can be more effectively controlled at about 0.5 μm or less, which is said to be good.

【0033】[0033]

【実施例】次に、実施例並びに比較例により、本発明を
説明する。尚、以下の実施例並びに比較例における粒子
の平均径は電子顕微鏡写真から測定した数値の平均値で
示したものであり、厚み及び板状比はBET法により測
定した比表面積値と上記平均径から求めた数値で示し
た。粒度分布の良否は電子顕微鏡観察の結果で示した。
Next, the present invention will be described with reference to examples and comparative examples. In the following Examples and Comparative Examples, the average diameter of the particles is indicated by an average value of numerical values measured from an electron micrograph, and the thickness and plate ratio are the specific surface area value measured by the BET method and the average diameter. It was shown by the numerical value obtained from. The quality of the particle size distribution was shown by the result of observation with an electron microscope.

【0034】配向度は、下記試験片を用い、X線回折に
より求めたヘマタイトの110面におけるX線ピーク強
度I(110) に対するヘマタイトの006面におけるX線
ピーク強度I(006) の比で示した。この値が大きくなる
程配向度が優れていることを示す。
The degree of orientation is shown by the ratio of the X-ray peak intensity I (006) on the 006 plane of hematite to the X-ray peak intensity I (110) on the 110 plane of hematite obtained by X-ray diffraction using the following test piece. Was. The larger this value is, the better the degree of orientation is.

【0035】測定用試料片は、ヘマタイト粒子粉末0.
5gとヒマシ油1.0ccをフーバー式マーラーで練っ
てペースト状とし、このペーストにクリヤラッカー4.
5gを加え混練し塗料化して、キャストコート紙上に6
milのアプリケータを用いて塗布することによって得
た。
The measurement sample piece was prepared by using a hematite particle powder of 0.1%.
5 g and 1.0 cc of castor oil are kneaded with a Hoover-type muller to form a paste.
Add 5 g, knead it to make a paint, and put 6 g on cast coated paper.
Obtained by application using a mil applicator.

【0036】<板状ヘマタイト粒子粉末の製造法> 実施例1〜5 比較例1〜2; 実施例1 針状α−FeOOH粒子(長軸1μm、軸比20:1、
BET比表面積60m2 /g)を温度400℃で1時間
加熱脱水して得られた多結晶の針状ヘマタイト粒子(長
軸1μm、軸比20:1、BET比表面積80m2
g、結晶子サイズ80Å)を種晶とし、該種晶0.00
44mol(α−FeOOHに対し0.55mol%に
該当する。)及びα−FeOOH(長軸3μm、軸比1
0、BET比表面積20m2 /g)0.8molとNa
OH0.3molとを混合して得られた0.3Nのアル
カリ性懸濁液をオートクレーブ中で245℃まで加熱
し、機械的に攪拌しつつこの温度に0.5時間保持し、
暗紫色沈澱を生成させた。室温までに冷却後、暗紫色沈
澱を濾別し、十分水洗した後乾燥した。得られた乾燥粒
子粉末は、X線回折の結果、ヘマタイト粒子であり、電
子顕微鏡観察の結果、板面径6μm、厚み0.31μm
であって板状比が19であり、面内方向で粒子相互が重
なり合って連続的に配列していた。また、粒度分布は狭
いものであり、配向度は40と配向性の優れたものであ
った。
<Method for Producing Plate-like Hematite Particle Powder> Examples 1-5 Comparative Examples 1-2; Example 1 Acicular α-FeOOH particles (major axis 1 μm, axis ratio 20: 1,
Acicular hematite particles (major axis 1μm polycrystalline obtained a BET specific surface area of 60 m 2 / g) for 1 hour heated and dehydrated at a temperature 400 ° C., axial ratio 20: 1, a BET specific surface area of 80 m 2 /
g, with a crystallite size of 80 °) as a seed crystal.
44 mol (corresponding to 0.55 mol% with respect to α-FeOOH) and α-FeOOH (long axis 3 μm, axial ratio 1)
0, BET specific surface area 20 m 2 / g) 0.8 mol and Na
0.3 N alkaline suspension obtained by mixing with 0.3 mol of OH was heated to 245 ° C. in an autoclave and kept at this temperature for 0.5 hour while mechanically stirring,
A dark purple precipitate formed. After cooling to room temperature, the dark purple precipitate was filtered off, washed thoroughly with water and dried. The obtained dry particle powder is a hematite particle as a result of X-ray diffraction, and as a result of observation with an electron microscope, a plate surface diameter of 6 μm and a thickness of 0.31 μm
In this case, the plate-like ratio was 19, and the particles overlapped each other in the in-plane direction and were continuously arranged. Further, the particle size distribution was narrow, and the degree of orientation was 40, which was excellent in orientation.

【0037】実施例2 種晶の使用量を0.0019mol(α−FeOOHに
対し0.27mol%に該当する。)、α−FeOOH
の使用量を0.7mol、NaOHの使用量を0.4m
olとし、水熱処理を温度240℃で0.75時間行な
った以外は実施例1と同様にして暗紫色粒子粉末を得
た。得られた乾燥粒子粉末は、X線回折の結果、ヘマタ
イト粒子であり、電子顕微鏡観察の結果、板面径8μ
m、厚み0.30μmであって板状比が26.7であ
り、面内方向で粒子相互が重なり合って連続的に配列し
ていた。また、粒度分布は狭いものであり、配向度は4
5と配向性の優れたものであった。
Example 2 The amount of the seed crystal used was 0.0019 mol (corresponding to 0.27 mol% based on α-FeOOH), α-FeOOH
0.7mol, NaOH 0.4m
ol, and a dark purple particle powder was obtained in the same manner as in Example 1 except that the hydrothermal treatment was performed at a temperature of 240 ° C. for 0.75 hours. The obtained dry particle powder was a hematite particle as a result of X-ray diffraction.
m, the thickness was 0.30 μm, the plate-like ratio was 26.7, and the particles overlapped in the in-plane direction and were continuously arranged. The particle size distribution is narrow, and the degree of orientation is 4
5 and excellent orientation.

【0038】実施例3 針状α−FeOOH粒子(長軸1.5μm、軸比15、
BET比表面積35m 2 /g)を温度400℃で1時間
加熱脱水して得られた多結晶の針状ヘマタイト粒子(長
軸1.5μm、軸比15、BET比表面積45m2
g、結晶子サイズ110Å)を種晶とし、該種晶0.0
0018mol(α−FeOOHに対し0.023mo
l%に該当する。)及びα−FeOOH(長軸2.5μ
m、軸比12、BET比表面積22m2 /g)0.8m
olとNaOH0.2molとを混合して得られた0.
2Nのアルカリ性懸濁液をオートクレーブ中で255℃
まで加熱し、機械的に攪拌しつつこの温度に0.5時間
保持し、暗紫色沈澱を生成させた。室温までに冷却後、
暗紫色沈澱を濾別し、十分水洗した後乾燥した。得られ
た乾燥粒子粉末は、X線回折の結果、ヘマタイト粒子で
あり、電子顕微鏡観察の結果、板面径7μm、厚み0.
39μmであって板状比が18であり、面内方向で粒子
相互が重なり合って連続的に配列していた。また、粒度
分布は狭いものであり、配向度は35と配向性の優れた
ものであった。
Example 3 Acicular α-FeOOH particles (long axis 1.5 μm, axial ratio 15,
BET specific surface area 35m Two/ G) at 400 ° C for 1 hour
Polycrystalline needle-like hematite particles (length
1.5 μm axis, axial ratio 15, BET specific surface area 45 mTwo/
g, crystallite size of 110 °) as a seed crystal.
0018 mol (0.023 mol based on α-FeOOH)
1%. ) And α-FeOOH (long axis 2.5μ)
m, axial ratio 12, BET specific surface area 22mTwo/ G) 0.8m
ol and 0.2 mol of NaOH obtained by mixing.
2N alkaline suspension at 255 ° C. in autoclave
Heat to this temperature for 0.5 hour with mechanical stirring
Retained, forming a dark purple precipitate. After cooling to room temperature,
The dark purple precipitate was filtered off, washed thoroughly with water and dried. Obtained
X-ray diffraction shows that the dried powder
As a result of observation with an electron microscope, the plate surface diameter was 7 μm and the thickness was 0.
39 μm, the plate-like ratio is 18, and particles in the in-plane direction
They overlapped each other and were arranged continuously. Also, the particle size
The distribution is narrow and the degree of orientation is 35, which is excellent in orientation.
Was something.

【0039】実施例4 針状α−FeOOH粒子(長軸0.5μm、軸比10:
1、BET比表面積110m2 /g、Ti含有 Ti/
Ti+Fe=15mol%)を温度500℃で30分間
加熱脱水して得られた多結晶のTi含有針状ヘマタイト
粒子(長軸0.5μm、軸比10:1、BET比表面積
50m2 /g、結晶子サイズ90Å)を種晶とし、該種
晶0.0044mol(α−FeOOHに対し、0.5
5mol%に該当する。)及びα−FeOOH(長軸3
μm、軸比10:1、BET比表面積20m2 /g)
0.8molとNaOH 0.3molとを混合して得
られた0.3Nアルカリ性懸濁液をオートクレーブ中で
245℃まで加熱し、機械的に攪拌しつつこの温度に
0.5時間保持し、暗紫色沈澱を生成させた。室温まで
に冷却後、暗紫色沈澱を濾別し、十分水洗した後乾燥し
た。得られた乾燥粒子粉末は、X線回折の結果、ヘマタ
イト粒子であり、図4に示す電子顕微鏡写真(×150
0)に示す通り、板面径6μm、厚み0.21μmであ
って板状比が29であり、面内方向で粒子相互が重なり
合って連続的に配列していた。また、粒度分布は狭いも
のであり、配向度は53と配向性の優れたものであっ
た。
Example 4 Acicular α-FeOOH particles (major axis: 0.5 μm, axial ratio: 10:
1. BET specific surface area 110 m 2 / g, Ti containing Ti /
Polycrystalline Ti-containing needle-like hematite particles (major axis: 0.5 μm, axis ratio: 10: 1, BET specific surface area: 50 m 2 / g, crystal obtained by heating and dehydrating Ti + Fe = 15 mol%) at a temperature of 500 ° C. for 30 minutes. (Crystal size 90 °) was used as a seed crystal, and the seed crystal was 0.0044 mol (0.5 with respect to α-FeOOH).
This corresponds to 5 mol%. ) And α-FeOOH (long axis 3)
μm, axial ratio 10: 1, BET specific surface area 20 m 2 / g)
A 0.3 N alkaline suspension obtained by mixing 0.8 mol with 0.3 mol of NaOH is heated to 245 ° C. in an autoclave and kept at this temperature for 0.5 hour while mechanically stirring to obtain a dark purple A precipitate formed. After cooling to room temperature, the dark purple precipitate was filtered off, washed thoroughly with water and dried. As a result of X-ray diffraction, the obtained dry particle powder was a hematite particle, and was observed by an electron micrograph (× 150) shown in FIG.
As shown in (0), the plate surface diameter was 6 μm, the thickness was 0.21 μm, the plate ratio was 29, and the particles were overlapped and arranged continuously in the in-plane direction. Further, the particle size distribution was narrow, and the degree of orientation was 53, which was excellent.

【0040】実施例5 針状α−FeOOH粒子(長軸0.5μm、軸比10:
1、BET比表面積110m2 /g、Ti含有 Ti/
Ti+Fe=15mol%)を温度500℃で30分間
加熱脱水して得られた多結晶のTi含有針状ヘマタイト
粒子(長軸0.5μm、軸比10:1、BET比表面積
50m2 /g、結晶子サイズ90Å)を種晶とし、該種
晶0.0018mol(α−FeOOHに対し、0.2
7mol%に該当する。)及びFeCl3 0.7mo
lとNaOH 0.4molとを混合して得られた0.
7Nアルカリ性懸濁液をオートクレーブ中で230℃ま
で加熱し、機械的に攪拌しつつこの温度に1時間保持
し、暗紫色沈澱を生成させた。室温までに冷却後、暗紫
色沈澱を濾別し、十分水洗した後乾燥した。得られた乾
燥粒子粉末は、X線回折の結果、ヘマタイト粒子であ
り、電子顕微鏡観察の結果、板面径7μm、厚み0.2
8μmであって板状比が25であり、面内方向で粒子相
互が重なり合って連続的に配列していた。また、粒度分
布は狭いものであり、配向度は41と配向性の優れたも
のであった。
Example 5 Acicular α-FeOOH particles (major axis: 0.5 μm, axial ratio: 10:
1. BET specific surface area 110 m 2 / g, Ti containing Ti /
Polycrystalline Ti-containing needle-like hematite particles (major axis: 0.5 μm, axis ratio: 10: 1, BET specific surface area: 50 m 2 / g, crystal obtained by heating and dehydrating Ti + Fe = 15 mol%) at a temperature of 500 ° C. for 30 minutes. (Crystal size 90 °) was used as a seed crystal, and the seed crystal was 0.0018 mol (0.2% based on α-FeOOH).
This corresponds to 7 mol%. ) And FeCl 3 0.7mo
and 0.1 mol of NaOH obtained by mixing 0.4 mol of NaOH with 0.4 mol of NaOH.
The 7N alkaline suspension was heated to 230 ° C. in an autoclave and held at this temperature for 1 hour with mechanical stirring to produce a dark purple precipitate. After cooling to room temperature, the dark purple precipitate was filtered off, washed thoroughly with water and dried. The obtained dry particle powder was a hematite particle as a result of X-ray diffraction, and as a result of observation with an electron microscope, the plate surface diameter was 7 μm and the thickness was 0.2.
The particle size was 8 μm, the plate ratio was 25, and the particles overlapped in the in-plane direction and were continuously arranged. In addition, the particle size distribution was narrow, and the degree of orientation was 41, which was excellent.

【0041】比較例1 種晶を添加しなかった以外は、実施例4と同様にして暗
紫色沈澱を生成させた。室温までに冷却後、暗紫色沈澱
を濾別し、十分水洗した後乾燥した。得られた乾燥粒子
粉末は、X線回折の結果、ヘマタイト粒子であり、図5
に示す電子顕微鏡写真(×1000)に示す通り、板面
径8μm、厚み1.0μmであって板状比8であった。
また、粒度分布は優れたものとは言い難く、粒子の厚み
が厚いことによって個々の板状粒子の向きが一様ではな
く、しかも、個々の粒子が独立して存在しており、その
結果、配向度が5と配向性が悪いものであった。
Comparative Example 1 A dark purple precipitate was formed in the same manner as in Example 4 except that no seed crystal was added. After cooling to room temperature, the dark purple precipitate was filtered off, washed thoroughly with water and dried. As a result of X-ray diffraction, the obtained dry particle powder was a hematite particle.
As shown in the electron micrograph (× 1000) shown in FIG. 1, the plate surface diameter was 8 μm, the thickness was 1.0 μm, and the plate ratio was 8.
In addition, the particle size distribution is hard to say excellent, due to the large thickness of the particles, the direction of the individual plate-like particles is not uniform, and furthermore, the individual particles exist independently, as a result, The degree of orientation was 5 and the orientation was poor.

【0042】比較例2 種晶として板状ヘマタイト粒子(板面径5μm、厚み
0.6μm、板状比8)を用いた以外は、実施例4と同
様にして暗紫色沈澱を生成させた。室温までに冷却後、
暗紫色沈澱を濾別し、十分水洗した後乾燥した。得られ
た乾燥粒子粉末は、X線回折の結果、ヘマタイト粒子で
あり、図6に示す電子顕微鏡写真(×1000)に示す
通り、板面径9μm、厚み0.7μmであって板状比1
3であった。また、粒度が不均斉であり個々の粒子が独
立して存在しており、その結果、配向度が7と配向性が
悪いものであった。
Comparative Example 2 A dark purple precipitate was formed in the same manner as in Example 4, except that plate-like hematite particles (plate diameter: 5 μm, thickness: 0.6 μm, plate ratio: 8) were used as seed crystals. After cooling to room temperature,
The dark purple precipitate was filtered off, washed thoroughly with water and dried. As a result of X-ray diffraction, the obtained dry particle powder was a hematite particle, and had a plate surface diameter of 9 μm, a thickness of 0.7 μm and a plate ratio of 1 as shown in the electron micrograph (× 1000) shown in FIG.
It was 3. In addition, the particle size was uneven and individual particles were present independently. As a result, the degree of orientation was 7 and the orientation was poor.

【0043】<板状マグネタイト粒子粉末の製造法> 実施例6 実施例3で得られた板状ヘマタイト粒子粉末30gをH
2 ガスを毎分0.5lの割合で通気して還元温度380
℃で還元して板状マグネタイト粒子粉末を得た。得られ
た板状マグネタイト粒子は、電子顕微鏡観察の結果、板
面径7μm、厚み0.39μmであって板状比が18で
あり、面内方向で粒子相互が重なり合って連続的に配列
していた。また、粒度分布は狭いものであり、配向性は
走査型電子顕微鏡観察の結果、優れたものであった。
<Method for Producing Plate-like Magnetite Particle Powder> Example 6 30 g of the plate-like hematite particle powder obtained in Example 3 was H
Two gases were introduced at a rate of 0.5 l / min to reduce the temperature to 380.
It was reduced at ℃ to obtain a plate-like magnetite particle powder. As a result of observation with an electron microscope, the obtained plate-like magnetite particles had a plate surface diameter of 7 μm, a thickness of 0.39 μm, and a plate ratio of 18, and the particles were overlapped in the in-plane direction and continuously arranged. Was. The particle size distribution was narrow, and the orientation was excellent as a result of observation with a scanning electron microscope.

【0044】実施例7 実施例1で得られた板状ヘマタイト粒子粉末30gをH
2 ガスを毎分0.5lの割合で通気して還元温度380
℃で還元して板状マグネタイト粒子粉末を得た。得られ
た板状マグネタイト粒子は、電子顕微鏡観察の結果、板
面径6μm、厚み0.30μmであって板状比が20で
あり、面内方向で粒子相互が重なり合って連続的に配列
していた。また、粒度分布は狭いものであり、配向性は
走査型電子顕微鏡観察の結果、優れたものであった。
Example 7 30 g of the plate-like hematite particle powder obtained in Example 1 was mixed with H
Two gases were introduced at a rate of 0.5 l / min to reduce the temperature to 380.
It was reduced at ℃ to obtain a plate-like magnetite particle powder. As a result of observation with an electron microscope, the obtained plate-like magnetite particles had a plate surface diameter of 6 μm, a thickness of 0.30 μm, and a plate ratio of 20, and the particles were overlapped in the in-plane direction and arranged continuously. Was. The particle size distribution was narrow, and the orientation was excellent as a result of observation with a scanning electron microscope.

【0045】<板状マグヘマイト粒子粉末の製造法> 実施例8 実施例7で得られた板状マグネタイト粒子粉末20gを
空気中280℃で30分間酸化して板状マグヘマイト粒
子粉末を得た。得られた板状マグヘマイト粒子は、電子
顕微鏡観察の結果、板面径6μm、厚み0.31μmで
あって板状比が19であり、面内方向で粒子相互が重な
り合って連続的に配列していた。また、粒度分布は狭い
ものであり、配向性は走査型電子顕微鏡観察の結果、優
れたものであった。
<Production method of plate-like maghemite particle powder> Example 8 20 g of the plate-like magnetite particle powder obtained in Example 7 was oxidized in air at 280 ° C for 30 minutes to obtain plate-like maghemite particle powder. As a result of observation with an electron microscope, the obtained plate-like maghemite particles had a plate surface diameter of 6 μm, a thickness of 0.31 μm, and a plate-like ratio of 19, and were continuously arranged with the particles overlapping in the in-plane direction. Was. The particle size distribution was narrow, and the orientation was excellent as a result of observation with a scanning electron microscope.

【0046】[0046]

【表1】 [Table 1]

【0047】[0047]

【発明の効果】本発明に係る板状酸化鉄粒子粉末の製造
法によれば、前出実施例に示した通り、粒度が均斉であ
って配向性が優れており、しかも粒子の厚みが制御され
た板状酸化鉄粒子粉末が得られるから、ビヒクルや樹脂
への分散性、配向性及びなじみが優れているので、塗料
用、樹脂用、印刷インキ用、化粧品用、樹脂成形物用等
の着色顔料、電磁波吸収用、シールド用、制振用、防音
用、磁性トナー用磁気記録用等の材料として好適であ
る。
According to the method for producing plate-like iron oxide particles according to the present invention, the particle size is uniform, the orientation is excellent, and the thickness of the particles is controlled, as shown in the above examples. The obtained plate-like iron oxide particle powder has excellent dispersibility, orientation and conformability to vehicles and resins, and is suitable for paints, resins, printing inks, cosmetics, resin moldings, etc. It is suitable as a coloring pigment, a material for electromagnetic wave absorption, shielding, vibration suppression, soundproofing, magnetic recording for magnetic toner, and the like.

【0048】また、本発明に係る板状酸化鉄粒子粉末
は、前出実施例に示した通り、板状粒子のほぼ中央付近
に細長い小さな孔を有しており、これら粒子粉末を用い
て塗膜を形成したり成形物を製造した場合には、粒子の
孔の部分に樹脂が混入して、塗膜の強化や剥離防止が期
待され、しかも、粒子中の上記孔は小さい為板状粒子の
光輝感を害することもない。
Further, the plate-like iron oxide particles according to the present invention, as shown in the above-described embodiment, have elongated small holes near the center of the plate-like particles. When a film is formed or a molded product is produced, the resin is mixed into the pores of the particles, thereby strengthening and preventing peeling of the coating film. It does not impair the luminosity of the camera.

【図面の簡単な説明】[Brief description of the drawings]

【図1】生成した板状ヘマタイト粒子粉末の厚みと反応
温度との関係を示したものである。
FIG. 1 shows the relationship between the thickness of the produced plate-like hematite particle powder and the reaction temperature.

【図2】生成した板状ヘマタイト粒子粉末の厚みとアル
カリ濃度との関係を示したものである。
FIG. 2 shows the relationship between the thickness of the produced plate-like hematite particles and the alkali concentration.

【図3】生成した板状ヘマタイト粒子粉末の厚みと種晶
として使用した針状ヘマタイト粒子の厚みとの関係を示
したものである。
FIG. 3 shows the relationship between the thickness of the produced plate-like hematite particle powder and the thickness of acicular hematite particles used as seed crystals.

【図4】実施例4で得られた板状ヘマタイト粒子粉末の
粒子構造を示す電子顕微鏡写真(×1500)である。
FIG. 4 is an electron micrograph (× 1500) showing the particle structure of the plate-like hematite particle powder obtained in Example 4.

【図5】比較例1で得られた板状ヘマタイト粒子粉末の
粒子構造を示す電子顕微鏡写真(×1000)である。
FIG. 5 is an electron micrograph (× 1000) showing the particle structure of the plate-like hematite particle powder obtained in Comparative Example 1.

【図6】比較例2で得られた板状ヘマタイト粒子粉末の
粒子構造を示す電子顕微鏡写真(×1000)である。
FIG. 6 is an electron micrograph (× 1000) showing the particle structure of the plate-like hematite particle powder obtained in Comparative Example 2.

Claims (2)

(57)【特許請求の範囲】(57) [Claims] 【請求項1】 含水酸化第二鉄粒子又は第二鉄塩を含む
pH11以上のアルカリ性懸濁液を水熱処理することに
よって板状ヘマタイト粒子粉末を生成させる方法におい
て、前記アルカリ性懸濁液中にあらかじめ種晶として針
状含水酸化第二鉄粒子を加熱処理して得られる針状ヘマ
タイト粒子を添加すると共に、pHを11以上とし、且
つ、アルカリ濃度を0.3〜0.7Nの範囲とし、次い
150〜330℃の温度範囲で水熱処理することによ
厚みが0.5μm以下の板状ヘマタイト粒子を生成さ
せることを特徴とする板状酸化鉄粒子粉末の製造法。
1. A method for producing a plate-like hematite particle powder by hydrothermally treating an alkaline suspension having a pH of 11 or more containing hydrous ferric oxide particles or a ferric salt. Needle-like hematite particles obtained by heat-treating needle-like hydrous ferric oxide particles as seed crystals are added , the pH is adjusted to 11 or more, and
First, a plate-like hematite particle having a thickness of 0.5 μm or less is formed by setting the alkali concentration in the range of 0.3 to 0.7 N and then performing a hydrothermal treatment in a temperature range of 150 to 330 ° C. A method for producing a plate-like iron oxide particle powder, comprising:
【請求項2】 請求項1で得られた板状ヘマタイト粒子
を加熱還元して板状マグネタイト粒子とするか、又は、
更に酸化して板状マグヘマイト粒子とすることを特徴と
する板状酸化鉄粒子粉末の製造法。
2. The heat treatment of the plate-like hematite particles obtained in claim 1 to form plate-like magnetite particles, or
A method for producing plate-like iron oxide particles, which is further oxidized into plate-like maghemite particles.
JP4224764A 1992-07-31 1992-07-31 Production method of plate-like iron oxide particles Expired - Fee Related JP3045207B2 (en)

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Application Number Priority Date Filing Date Title
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JP3045207B2 true JP3045207B2 (en) 2000-05-29

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* Cited by examiner, † Cited by third party
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JP2824203B2 (en) * 1994-03-18 1998-11-11 大倉工業株式会社 Plastic trash bags
KR101026361B1 (en) * 2008-07-03 2011-04-05 씨큐브 주식회사 Method of manufacturing hematite platelets, hematite platelets and hematite platelets pigment fabricated using thereof
CN103534367A (en) 2011-03-18 2014-01-22 奥贝特铝业有限公司 Processes for recovering rare earth elements from aluminum-bearing materials
RU2013157943A (en) * 2011-06-03 2015-07-20 Орбит Элюминэ Инк. HEMATITIS METHOD
BR112014001239A2 (en) * 2011-07-18 2017-07-18 Orbite Aluminae Inc method for separating iron ions from aluminum ions contained in an acidic composition and method for treating an acidic composition comprising iron ions and aluminum ions
US9382600B2 (en) 2011-09-16 2016-07-05 Orbite Technologies Inc. Processes for preparing alumina and various other products
CN103601253B (en) * 2013-11-05 2014-12-24 陕西科技大学 Disk type alpha-Fe2O3 photocatalyst and preparation method and application thereof
CN105289456B (en) * 2015-09-29 2019-09-24 合肥学院 A kind of superparamagnetic Fe3O4The preparation method and application of nano material

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