JPH05294626A - White magnetic powder and its production - Google Patents

White magnetic powder and its production

Info

Publication number
JPH05294626A
JPH05294626A JP9753692A JP9753692A JPH05294626A JP H05294626 A JPH05294626 A JP H05294626A JP 9753692 A JP9753692 A JP 9753692A JP 9753692 A JP9753692 A JP 9753692A JP H05294626 A JPH05294626 A JP H05294626A
Authority
JP
Japan
Prior art keywords
magnetic
titanium oxide
powder
particle powder
white
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
JP9753692A
Other languages
Japanese (ja)
Other versions
JP3290200B2 (en
Inventor
Yoshishige Koma
佳茂 駒
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Kanto Denka Kogyo Co Ltd
Original Assignee
Kanto Denka Kogyo Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Kanto Denka Kogyo Co Ltd filed Critical Kanto Denka Kogyo Co Ltd
Priority to JP09753692A priority Critical patent/JP3290200B2/en
Publication of JPH05294626A publication Critical patent/JPH05294626A/en
Application granted granted Critical
Publication of JP3290200B2 publication Critical patent/JP3290200B2/en
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

Links

Abstract

PURPOSE:To provide white magnetic particle powder having magnetic characteristics suitable for magnetic toner. CONSTITUTION:The title white magnetic powder is characterized by depositing magnetic oxide iron onto titanium oxide particle powder using the titanium oxide particle powder as a nuclei. The process for the production of the white magnetic powder comprises the steps of suspending the titanium oxide particle powder in an aqueous solution containing a salt of iron (II) and a salt of iron (III), heating the suspension to 40-90 deg.C while stirring, adding an alkali hydroxide to the suspension till pH becomes 8-9 and depositing the magnetic iron oxide onto the titanium oxide powder using the titanium oxide particle powder as a nuclei.

Description

【発明の詳細な説明】Detailed Description of the Invention

【産業上の利用分野】本発明は、白色磁性粉末、詳しく
は、磁性カラートナーや着色磁性顔料の原料用として有
用な白色磁性粉末及びその製造方法に関するものであ
る。
BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to white magnetic powder, and more particularly to white magnetic powder useful as a raw material for magnetic color toners and colored magnetic pigments, and a method for producing the same.

【従来の技術及び発明が解決しようとする課題】従来よ
りトナーとキャリアとを用いるカラー電子写真法におい
て、静電潜像を白色に現像する現像剤として、白色顔
料、例えば酸化チタン、硫酸バリウム、酸化亜鉛、硫酸
亜鉛等の単体もしくはこれらを2種組み合わせた混合物
をアクリル樹脂、スチレン−アクリル共重合樹脂、フッ
素樹脂等でコーティングしたものが用いられてきてい
る。しかし、この2成分系の電子写真法は比較的安定し
た画像が得られるすぐれた方法であるものの、反面キャ
リアの劣化、トナーとキャリアとの混合比の変動といっ
た欠点も有している。かかる欠点を回避するために、ト
ナーのみからなる一成分系現像剤を用いる現像方法が種
々提案されているが、その中でも磁性トナー粒子からな
る現像剤を用いる方法がすぐれていると言える。この一
成分系現像剤で静電潜像を白色に現像するためには、磁
性を有する白色のトナーを使用する必要があるが、前述
の白色顔料には磁性を有するものが無く、何らかの手段
でこれらに磁性を付与する必要がある。その手段とし
て、代表的な磁性体であるγ−Fe2O3 、Fe3O4 等を、白
色顔料を含む樹脂でコートする方法が考えられる。しか
し、この方法では、磁性体の色が強く出るために、白色
とするには白色顔料を含む樹脂を大量にコートしなけれ
ばならず、そのため必要とする磁気特性が得られない。
従って、磁気特性を低下させることなく白色の磁性粒子
粉末を得る方法の開発が望まれている。また、磁性を有
する白色粒子粉末は、着色磁性顔料用としても用途が開
ける可能性がある。従って、本発明の目的は、磁性カラ
ートナー用に適した磁気特性を有する白色の磁性粒子粉
末を提供することにある。
2. Description of the Related Art Conventionally, in a color electrophotographic method using a toner and a carrier, a white pigment such as titanium oxide or barium sulfate is used as a developer for developing an electrostatic latent image into white. A single substance such as zinc oxide or zinc sulfate or a mixture of two or more thereof coated with an acrylic resin, a styrene-acrylic copolymer resin, a fluororesin or the like has been used. However, although this two-component electrophotographic method is an excellent method capable of obtaining a relatively stable image, it also has drawbacks such as deterioration of the carrier and fluctuation of the mixing ratio of the toner and the carrier. In order to avoid such drawbacks, various developing methods using a one-component developer containing only toner have been proposed, and among them, the method using a developer containing magnetic toner particles is said to be excellent. In order to develop an electrostatic latent image in white with this one-component developer, it is necessary to use a white toner having magnetism. It is necessary to impart magnetism to these. As a means therefor, a method of coating γ-Fe 2 O 3 , Fe 3 O 4, etc., which are typical magnetic materials, with a resin containing a white pigment is considered. However, in this method, since the color of the magnetic material is strong, a large amount of resin containing a white pigment must be coated to obtain a white color, and thus the required magnetic properties cannot be obtained.
Therefore, development of a method for obtaining white magnetic particle powder without deteriorating magnetic properties is desired. In addition, the magnetic white particle powder may be used for colored magnetic pigments. Therefore, it is an object of the present invention to provide a white magnetic particle powder having magnetic properties suitable for a magnetic color toner.

【課題を解決するための手段】本発明者は、鋭意研究し
た結果、酸化チタンに磁性酸化鉄を特定の温度及びpH
条件下で析出させることにより、上記目的が達成される
ことを知見した。本発明は、上記知見に基づいてなされ
たもので、酸化チタン粒子粉末を核として、該酸化チタ
ン粒子粉末に磁性酸化鉄を析出させたことを特徴とする
白色磁性粉末を提供するものである。また、本発明は、
本発明の白色磁性粉末の好ましい製造法として、第一鉄
塩及び第二鉄塩を含む水溶液中に酸化チタン粒子粉末を
懸濁させ、該懸濁液を攪拌しつつ40〜90℃に加熱
し、次いでpHが8〜9になるまで水酸化アルカリを添
加し、上記酸化チタン粒子粉末を核として、該酸化チタ
ン粒子粉末に磁性酸化鉄を析出させることを特徴とする
白色磁性粉末の製造方法を併せて提供するものである。
以下、本発明の白色磁性粉末を、本発明の製造法に基づ
いて詳述する。
As a result of earnest research, the present inventors have found that magnetic iron oxide is added to titanium oxide at a specific temperature and pH.
It was found that the above object can be achieved by precipitating under the conditions. The present invention has been made based on the above findings, and provides a white magnetic powder characterized in that magnetic iron oxide is deposited on the titanium oxide particle powder with the titanium oxide particle powder as the nucleus. Further, the present invention is
As a preferred method for producing the white magnetic powder of the present invention, the titanium oxide particle powder is suspended in an aqueous solution containing a ferrous salt and a ferric salt, and the suspension is heated to 40 to 90 ° C with stirring. Then, an alkali hydroxide is added until the pH becomes 8 to 9, and magnetic iron oxide is deposited on the titanium oxide particle powder with the titanium oxide particle powder as a core. It is also provided.
Hereinafter, the white magnetic powder of the present invention will be described in detail based on the production method of the present invention.

【0001】本発明の白色磁性粉末の製造法に使用され
る第一鉄塩及び第二鉄塩としては、塩化鉄、硫酸鉄及び
硝酸鉄等の第一鉄塩及び第二鉄塩が挙げられ、塩化鉄の
第一鉄塩及び第二鉄塩が特に好ましい。
Examples of the ferrous salt and ferric salt used in the method for producing the white magnetic powder of the present invention include ferrous and ferric salts such as iron chloride, iron sulfate and iron nitrate. Especially preferred are ferrous and ferric salts of iron chloride.

【0002】本発明の白色磁性粉末において、核となる
酸化チタン粒子粉末としては、本発明の白色磁性粉末の
用途を考慮すれば、粒径が細かい物が良く、通常、その
平均粒径は、0.1〜0.5μのものが好ましい。上記
酸化チタン粒子粉末は、上記第一鉄塩及び第二鉄塩の水
溶液中に、通常の方法で懸濁させる。
In the white magnetic powder of the present invention, as a titanium oxide particle powder serving as a core, a fine particle having a fine particle size is preferable in consideration of the use of the white magnetic powder of the present invention, and the average particle size thereof is usually It is preferably 0.1 to 0.5 μ. The titanium oxide particle powder is suspended in an aqueous solution of the ferrous salt and ferric salt by a conventional method.

【0003】懸濁させる酸化チタンの量に対する、上記
水溶液中の第一鉄塩又は第二鉄塩の量の比は、第一鉄塩
及び第二鉄塩共に、懸濁させる酸化チタンの量に対し、
好ましくは1.0〜20モル%である。第一鉄塩又は第
二鉄塩の量が、酸化チタンの量の1.0モル%未満であ
ると、飽和磁束密度(σS )及び保磁力(Hc ) が低く
なるおそれがあり、また、酸化チタンの量の20モル%
超であると、磁性粒子粉末が着色し易くなる。
The ratio of the amount of ferrous salt or ferric salt in the above-mentioned aqueous solution to the amount of titanium oxide to be suspended depends on the amount of titanium oxide to be suspended in both the ferrous salt and the ferric salt. On the other hand,
It is preferably 1.0 to 20 mol%. If the amount of the ferrous salt or ferric salt is less than 1.0 mol% of the amount of titanium oxide, the saturation magnetic flux density (σ S ) and the coercive force (H c ) may be low, and , 20 mol% of the amount of titanium oxide
If it is over, the magnetic particle powder will be easily colored.

【0004】また、本発明の白色磁性粉末の製造法にお
いて、上記第一鉄塩と第二鉄塩とは混合して使用され、
上記第一鉄塩と上記第二鉄塩との比(モル比)は、(前
者)/(後者)=1/0.1〜1/1とすることが好ま
しい。上記第一鉄塩と上記第二鉄塩とを混合して使用し
ない場合、例えば、上記第一鉄塩のみを使用した場合に
は、中和によって生成するのがFe3O4 のみになるので生
成物に黒味がつくので好ましくない。また、上記水溶液
中の第一鉄塩の濃度は、好ましくは0.025〜2.5
Mであり、第二鉄塩の濃度は、好ましくは0.005〜
0.25Mである。
Further, in the method for producing a white magnetic powder of the present invention, the ferrous salt and ferric salt are mixed and used,
The ratio (molar ratio) of the ferrous salt to the ferric salt is preferably (former) / (latter) = 1 / 0.1 to 1/1. When the ferrous salt and the ferric salt are not mixed and used, for example, when only the ferrous salt is used, only Fe 3 O 4 is produced by neutralization. It is not preferable because the product has a black tint. The concentration of the ferrous salt in the aqueous solution is preferably 0.025 to 2.5.
M, and the concentration of ferric salt is preferably 0.005
It is 0.25M.

【0005】本発明の白色磁性粉末の製造法において
は、上述の酸化チタンの懸濁液を攪拌しつつ40〜90
℃に加熱し、該温度範囲に保持して反応させる。反応温
度が40℃未満であると、反応速度が遅くなり実用的で
なく、また、90℃超であると、反応速度が速くなりす
ぎ、酸化チタン粒子粉末上に析出しない鉄酸化物が多
く、着色の原因になる。
In the method for producing the white magnetic powder of the present invention, the above-mentioned suspension of titanium oxide is stirred for 40 to 90 minutes.
The mixture is heated to 0 ° C. and kept in this temperature range for reaction. If the reaction temperature is lower than 40 ° C, the reaction rate becomes slow and not practical, and if it is higher than 90 ° C, the reaction rate becomes too fast, and many iron oxides do not precipitate on the titanium oxide particle powder, It causes coloring.

【0006】上記酸化チタンの懸濁液のpHは、水酸化
アルカリを、通常、水溶液として添加することにより、
8〜9に調整される。これにより、上記酸化チタン粒子
粉末に磁性酸化鉄が析出する。本発明の白色磁性粉末に
おける、上記酸化チタン粒子粉末(核)に析出する磁性
酸化鉄としては、γ−Fe2O3 、Fe3O4 等が挙げられ、上
記pHが8未満であると、α−Fe2O3 の生成が多くな
り、生成物の磁気特性が低下するため好ましくなく、上
記pHが9超であると、Fe3O4 の生成量が多くなり、生
成物に黒味がでてくるため好ましくない。尚、上述のよ
うに水酸化アルカリを添加する際、液温は、通常、上記
温度範囲に保持される。
The pH of the titanium oxide suspension can be adjusted by adding an alkali hydroxide, usually as an aqueous solution.
Adjusted to 8-9. As a result, magnetic iron oxide is deposited on the titanium oxide particle powder. In the white magnetic powder of the present invention, examples of the magnetic iron oxide deposited on the titanium oxide particle powder (nucleus) include γ-Fe 2 O 3 and Fe 3 O 4 , and the pH is less than 8. This is not preferable because the amount of α-Fe 2 O 3 produced is large and the magnetic properties of the product deteriorate, and when the pH is above 9, the amount of Fe 3 O 4 produced is large and the product has a black tint. It is not preferable because it comes out. When the alkali hydroxide is added as described above, the liquid temperature is usually maintained in the above temperature range.

【0007】以上の方法によって製造される白色磁性粉
末の平均粒径は、通常、0.2〜2.0μ程度、Hcは
10〜100Oe程度、また、σs は3〜10emu/
g程度であり、磁性カラートナーとして有用であり、ま
た、着色磁性顔料用としても用途が期待されるものであ
る。
The average particle size of the white magnetic powder produced by the above method is usually about 0.2 to 2.0 μ, Hc is about 10 to 100 Oe, and σ s is 3 to 10 emu /.
Since it is about g, it is useful as a magnetic color toner, and is expected to be used as a coloring magnetic pigment.

【0008】[0008]

【実施例】以下に、実施例を比較例とともに挙げ、本発
明の白色磁性粉末を具体的に説明する。
EXAMPLES The white magnetic powder of the present invention will be specifically described below with reference to Examples and Comparative Examples.

【0009】(実施例1〜3)純水200mlに所定量
(〔表1〕参照)の塩化第一鉄及び塩化第二鉄を加え、
攪拌しながら所定の温度(〔表1〕参照)になるまで加
熱し、酸化チタン粒子粉末(平均粒径0.3μ、純度9
9.8%)を10g(0.125モル)添加して懸濁さ
せた後、上記温度に保ちながら10分間攪拌を継続し、
次いで攪拌しながら0.5Nの苛性ソーダ水溶液を、所
定のpH(〔表1〕参照)になるまで滴下し、さらに攪
拌を続けて30分間維持した後、生成物を濾過し、乾燥
した。得られた磁性粒子粉末の磁気特性及び外観を次の
〔表1〕に示した。
Examples 1 to 3 A predetermined amount (see Table 1) of ferrous chloride and ferric chloride was added to 200 ml of pure water,
While stirring, the mixture was heated to a predetermined temperature (see [Table 1]), and titanium oxide particle powder (average particle size 0.3 µ, purity 9
10 g (0.125 mol) of 9.8%) was added and suspended, and then stirring was continued for 10 minutes while maintaining the above temperature,
Next, 0.5N aqueous caustic soda solution was added dropwise with stirring to a predetermined pH (see [Table 1]), and stirring was continued for 30 minutes, and then the product was filtered and dried. The magnetic properties and appearance of the obtained magnetic particle powder are shown in the following [Table 1].

【0010】(比較例1〜3)塩化第一鉄及び塩化第二
鉄の添加量、反応温度及びpHの条件を変えた他は、上
記実施例と同様にして磁性粒子粉末の製造を行った。製
造条件並びに得られた磁性粒子粉末の磁気特性及び外観
を次の〔表1〕に示した。
(Comparative Examples 1 to 3) Magnetic particle powders were produced in the same manner as in the above Examples except that the amounts of ferrous chloride and ferric chloride added, the reaction temperature and the pH were changed. .. The production conditions and the magnetic properties and appearance of the obtained magnetic particle powder are shown in the following [Table 1].

【0011】[0011]

【表1】 [Table 1]

【0012】[0012]

【発明の効果】本発明の白色磁性粉末は、磁性カラート
ナー用に適した磁気特性を有するものである。
The white magnetic powder of the present invention has magnetic properties suitable for magnetic color toners.

Claims (2)

【特許請求の範囲】[Claims] 【請求項1】 酸化チタン粒子粉末を核として、該酸化
チタン粒子粉末に磁性酸化鉄を析出させたことを特徴と
する白色磁性粉末。
1. A white magnetic powder characterized in that magnetic iron oxide is deposited on the titanium oxide particle powder by using the titanium oxide particle powder as a nucleus.
【請求項2】 第一鉄塩及び第二鉄塩を含む水溶液中に
酸化チタン粒子粉末を懸濁させ、該懸濁液を攪拌しつつ
40〜90℃に加熱し、次いでpHが8〜9になるまで
水酸化アルカリを添加し、上記酸化チタン粒子粉末を核
として、該酸化チタン粒子粉末に磁性酸化鉄を析出させ
ることを特徴とする白色磁性粉末の製造方法。
2. Titanium oxide particle powder is suspended in an aqueous solution containing a ferrous salt and a ferric salt, the suspension is heated to 40 to 90 ° C. with stirring, and then the pH is set to 8 to 9 A method for producing a white magnetic powder, characterized in that an alkali hydroxide is added until the above temperature is reached, and magnetic iron oxide is deposited on the titanium oxide particle powder by using the titanium oxide particle powder as a nucleus.
JP09753692A 1992-04-17 1992-04-17 Method for producing white magnetic powder Expired - Fee Related JP3290200B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP09753692A JP3290200B2 (en) 1992-04-17 1992-04-17 Method for producing white magnetic powder

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP09753692A JP3290200B2 (en) 1992-04-17 1992-04-17 Method for producing white magnetic powder

Publications (2)

Publication Number Publication Date
JPH05294626A true JPH05294626A (en) 1993-11-09
JP3290200B2 JP3290200B2 (en) 2002-06-10

Family

ID=14194976

Family Applications (1)

Application Number Title Priority Date Filing Date
JP09753692A Expired - Fee Related JP3290200B2 (en) 1992-04-17 1992-04-17 Method for producing white magnetic powder

Country Status (1)

Country Link
JP (1) JP3290200B2 (en)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2001017667A1 (en) * 1999-09-09 2001-03-15 Eichrom Technologies, Inc. Method of preparing metal oxide particles
JP2003002658A (en) * 2001-06-18 2003-01-08 Mitsui Mining & Smelting Co Ltd White magnetic powder
US10350933B2 (en) 2007-06-05 2019-07-16 Bank Of Canada Ink or toner compositions, methods of use, and products derived therefrom

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2001017667A1 (en) * 1999-09-09 2001-03-15 Eichrom Technologies, Inc. Method of preparing metal oxide particles
JP2003002658A (en) * 2001-06-18 2003-01-08 Mitsui Mining & Smelting Co Ltd White magnetic powder
JP4660678B2 (en) * 2001-06-18 2011-03-30 三井金属鉱業株式会社 White magnetic powder and method for producing the same
US10350933B2 (en) 2007-06-05 2019-07-16 Bank Of Canada Ink or toner compositions, methods of use, and products derived therefrom

Also Published As

Publication number Publication date
JP3290200B2 (en) 2002-06-10

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