JP3290200B2 - Method for producing white magnetic powder - Google Patents
Method for producing white magnetic powderInfo
- Publication number
- JP3290200B2 JP3290200B2 JP09753692A JP9753692A JP3290200B2 JP 3290200 B2 JP3290200 B2 JP 3290200B2 JP 09753692 A JP09753692 A JP 09753692A JP 9753692 A JP9753692 A JP 9753692A JP 3290200 B2 JP3290200 B2 JP 3290200B2
- Authority
- JP
- Japan
- Prior art keywords
- magnetic
- titanium oxide
- white
- powder
- magnetic powder
- 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.)
- Expired - Fee Related
Links
Description
【０００１】[0001]
【産業上の利用分野】本発明は、白色磁性粉末の製造方
法に関し、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の製造方法に関する
ものである。The present invention relates to a method for producing a white magnetic powder .
Respect the law, and more particularly to a method for producing a powder useful white magnetic powder as a raw material for a magnetic color toner or colored magnetic pigment.
【０００２】[0002]
【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。2. Description of the Related Art Conventionally, in color electrophotography using a toner and a carrier, a white pigment such as titanium oxide, barium sulfate, or the like is used as a developer for developing an electrostatic latent image into white. What has been used is one coated with an acrylic resin, a styrene-acrylic copolymer resin, a fluororesin or the like on a single substance such as zinc oxide or zinc sulfate or a mixture of two kinds thereof.
【０００３】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。[0003] However, although the two-component electrophotography is an excellent method for obtaining a relatively stable image,
On the other hand, it has disadvantages such as deterioration of the carrier and fluctuation of the mixing ratio between the toner and the carrier.
【０００４】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。In order to avoid such disadvantages, various developing methods using a one-component developer consisting of toner alone have been proposed. Among them, a method using a developer consisting of magnetic toner particles can be said to be superior. . In order to develop an electrostatic latent image into 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 a typical magnetic substance such as γ-Fe 2 O 3 or Fe 3 O 4 with a resin containing a white pigment can be considered. However, in this method, since the color of the magnetic material appears strongly, a large amount of a resin containing a white pigment must be coated to make it white.
Therefore, required magnetic characteristics cannot be obtained. Therefore, development of a method for obtaining white magnetic particle powder without deteriorating magnetic properties is desired. Further, the magnetic white particle powder may be used for coloring magnetic pigments.
【０００５】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粉末の製造方
法を提供することにある。It is therefore an object of the present invention, a white magnetic properties Powder manufacturing side of with magnetic properties suitable for a magnetic color toner
Is to provide a law .
【０００６】[0006]
【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。Means for Solving the Problems As a result of intensive studies, the present inventors have found that magnetic iron oxide is added to titanium oxide at a specific temperature and pH.
It has been found that the above object is achieved by precipitating under the conditions.
【０００７】本発明は、上記知見に基づいてなされたも
ので、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４０〜９
０℃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提供するものであ
る。[0007] The present invention has been made based on the above findings, suspending titanium oxide particles in an aqueous solution containing a first monoferric and ferric salts, while stirring the suspension 40 9
Heated to 0 ° C., and then added alkali hydroxide until the pH reached 8 to 9, with the titanium oxide particle powder as a core,
An object of the present invention is to provide a method for producing a white magnetic powder, comprising depositing magnetic iron oxide on the titanium oxide particles.
【０００８】[0008]
【発明の実施の形態】 以下、本発明の白色磁性粉末の製
造方法を詳述する。 DESCRIPTION OF THE PREFERRED EMBODIMENTS Hereinafter, detailed white magnetic Powder manufacturing <br/> manufacturing method of the present invention.
【０００９】本発明の白色磁性粉末の製造方法に使用さ
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。[0009] as a white magnetic powder ferrous and ferric salts to be used in the manufacture how of the present invention, include iron chloride, ferrous and ferric salts such as iron sulfate and iron nitrate And the ferrous and ferric salts of iron chloride are particularly preferred.
【００１０】本発明の白色磁性粉末の製造方法におい
て、核となる酸化チタン粒子粉末としては、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。[0010] White Te magnetic powder manufacturing process odor <br/> of the present invention, the titanium oxide particles as a core, in view of the use of white color magnetic powder, good ones particle size fine, usually,
The average particle size is preferably from 0.1 to 0.5 μm.
The titanium oxide particle powder is suspended in an aqueous solution of the ferrous salt and the ferric salt by an ordinary method.
【００１１】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 the ferrous salt or the ferric salt in the aqueous solution to the amount of the titanium oxide to be suspended is determined by the amount of the suspended titanium oxide in both the ferrous salt and the ferric salt. On the other hand,
Preferably it is 1.0 to 20 mol%. When the amount of the ferrous salt or the 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 more than 1, the magnetic particle powder is likely to be colored.
【００１２】また、本発明の白色磁性粉末の製造方法に
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〜
２．５Ｍであり、第二鉄塩の濃度は、好ましくは０．０
０５〜０．２５Ｍである。[0012] In the production how white magnetic powder of the present invention, the above ferrous salt and the ferric salt are used in admixture, the ratio of the ferrous salt and the ferric salt ( Molar ratio)
It is preferable that (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 generated by neutralization. It is not preferable because the product becomes blackish. The concentration of the ferrous salt in the aqueous solution is preferably 0.025 to
2.5M and the concentration of ferric salt is preferably 0.0
05-0.25M.
【００１３】本発明の白色磁性粉末の製造方法において
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。[0013] In the production how white the magnetic powder of the present invention, while stirring the suspension of titanium oxide above 40 to 90
C., and the reaction is carried out while maintaining the temperature. If the reaction temperature is less than 40 ° C., the reaction rate is not practical because it is slow, and if it is more than 90 ° C., the reaction rate is too fast and many iron oxides do not precipitate on the titanium oxide particle powder, It causes coloring.
【００１４】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。The pH of the titanium oxide suspension is adjusted by adding an alkali hydroxide, usually as an aqueous solution.
Adjusted to 8-9. Thereby, magnetic iron oxide precipitates on the titanium oxide particle powder.
【００１５】本発明の白色磁性粉末の製造方法におけ
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ｐ
Ｈ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。In the method for producing a white magnetic powder of the present invention, γ-Fe 2 O 3 , Fe 3 O 4, etc. are used as the magnetic iron oxide precipitated on the titanium oxide particle powder (nucleus). And p
When H is less than 8, the production of α-Fe 2 O 3 increases, and the magnetic properties of the product deteriorate.
Is more than 9, the production amount of Fe 3 O 4 is increased, and the product becomes blackish. When the alkali hydroxide is added as described above, the liquid temperature is usually kept in the above temperature range.
【００１６】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, usually, about 0.2 to 2.0 microns, Hc about 10～100Oe, also, sigma s is 3～10Emu /
g, which is useful as a magnetic color toner and is also expected to be used as a colored magnetic pigment.
【００１７】[0017]
【実施例】以下に、実施例を比較例とともに挙げ、本発
明の白色磁性粉末の製造方法を具体的に説明する。EXAMPLES Examples and comparative examples are described below to specifically describe the method for producing the white magnetic powder of the present invention.
【００１８】（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９９．８％）を１０ｇ（０．１２
５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 is added to 200 ml of pure water, and the mixture is stirred and heated to a predetermined temperature (see [Table 1]). And heated to 10 g of titanium oxide particles (average particle size: 0.3 μm, purity: 99.8%).
5 mol), and the mixture is suspended. Then, stirring is continued for 10 minutes while maintaining the above temperature, and then a 0.5N aqueous solution of caustic soda is added dropwise with stirring until a predetermined pH (see [Table 1]) is reached. After further stirring and maintaining for 30 minutes, the product was filtered and dried. The magnetic properties and appearance of the obtained magnetic particles are shown in the following [Table 1].
【００１９】（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) Addition amounts of ferrous chloride and ferric chloride, reaction temperature and pH
A magnetic particle powder was produced in the same manner as in the above example except that the conditions were changed. The production conditions and the magnetic properties and appearance of the obtained magnetic particles are shown in Table 1 below.
【００２０】[0020]
【表１】 [Table 1]
【００２１】[0021]
【発明の効果】本発明の製造方法により得られる白色磁
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 obtained by the production method of the present invention has magnetic properties suitable for a magnetic color toner.
Claims (1)
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。1. A 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. while stirring, and then the pH is adjusted to 8 to 9 ° C. A method for producing a white magnetic powder, comprising adding an alkali hydroxide to the above-mentioned titanium oxide particle powder to precipitate magnetic iron oxide on the titanium oxide particle powder.
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 JPH05294626A (en) | 1993-11-09 |
| JP3290200B2 true 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) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| AU1106801A (en) * | 1999-09-09 | 2001-04-10 | Eichrom Technologies, Inc. | Method of preparing metal oxide particles |
| 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 |
| HUE043241T2 (en) | 2007-06-05 | 2019-08-28 | Bank Of Canada | Ink or toner compositions, methods of use, and products derived therefrom |
-
1992
- 1992-04-17 JP JP09753692A patent/JP3290200B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPH05294626A (en) | 1993-11-09 |
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