JPS61102706A - Magnetic material to be treated and manufacture thereof - Google Patents
Magnetic material to be treated and manufacture thereofInfo
- Publication number
- JPS61102706A JPS61102706A JP59224129A JP22412984A JPS61102706A JP S61102706 A JPS61102706 A JP S61102706A JP 59224129 A JP59224129 A JP 59224129A JP 22412984 A JP22412984 A JP 22412984A JP S61102706 A JPS61102706 A JP S61102706A
- Authority
- JP
- Japan
- Prior art keywords
- magnetic
- treated
- magnetic material
- lipophilic
- deionized
- 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.)
- Pending
Links
Landscapes
- Hard Magnetic Materials (AREA)
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野]
本発明は、磁性トナー、磁性インク、磁性塗料、磁気テ
ープなどに用いられる粉粒状の磁性体及びその製造方法
に関する。DETAILED DESCRIPTION OF THE INVENTION [Field of Industrial Application] The present invention relates to a powdery magnetic material used in magnetic toner, magnetic ink, magnetic paint, magnetic tape, etc., and a method for producing the same.
〔従来の技術]
従来、磁性トナー、磁性インク、磁性塗料、磁気テープ
などには種々の磁性粉体が用いられている。[Prior Art] Conventionally, various magnetic powders have been used in magnetic toner, magnetic ink, magnetic paint, magnetic tape, and the like.
この代表例として1例えばFe30.やγ−Fe207
は種々の出発原料から合成され、−例として磁気材料と
して汎用されている針状γ−Fe207について述べる
と、a−Fe00H(Goethite)針状結晶を水
素気流中で脱水・還元してFe30Qとなし、これを空
気中で低温酸化する方法により製造される場合が多い。A representative example of this is 1, for example Fe30. or γ-Fe207
is synthesized from various starting materials. For example, in the case of acicular γ-Fe207, which is widely used as a magnetic material, a-Fe00H (Goethite) acicular crystals are dehydrated and reduced in a hydrogen stream to form Fe30Q. , is often produced by oxidizing it in air at a low temperature.
これらの反応過程における鉄イオンF、2+ 、 Fe
3+溶液などとアルカリ溶液との反応は、 Fe (O
H) 2やFe (OH) 3を生ずる単純な内容のよ
うに受取られやすいが、酸素を溶存する場合のこれらの
反応は非常に複雑で、この系統の反応には未だ不明な点
が多い。Iron ions F, 2+, Fe in these reaction processes
The reaction between 3+ solution etc. and alkaline solution is Fe (O
H) 2 and Fe (OH) 3 are produced, but these reactions are extremely complex when oxygen is dissolved, and there are still many points that are unclear about this type of reaction.
上記の原料たるGoethiteは塗料の黄色酸化鉄(
マルス黄)顔料〔橙黄色ないし黄色〕として汎用されて
おり、FaSOa水溶液とNaOH水溶液とを空気の存
在下にて種反応させ、種としてのα−Fe20.−H2
0の微結晶を生成させ1次に、鉄片とFeSO4水溶液
とを加え空気を吹き込みつつ主反応を行ない、水洗が過
の後、乾燥し得るのが通常の製法である。The raw material mentioned above, Goethite, is used in paints with yellow iron oxide (
Mars yellow) is widely used as a pigment (orange-yellow to yellow), and is produced by causing a seed reaction between an aqueous FaSOa solution and an aqueous NaOH solution in the presence of air to form α-Fe20. -H2
The usual manufacturing method is to first generate microcrystals of 0.0, then add an iron piece and an aqueous FeSO4 solution, carry out the main reaction while blowing air, wash with water, and then dry.
ところで上記原料のFe5Oaの入手経路であるが、現
在わが国においてはビックリング廃液またはチタン白製
造廃液から多量の硫酸第一鉄が副生されており、このV
tfftm−鉄溶液から反応条件を適当に組合せること
により、上記のGoethiteや黒色のFe30pの
鉄酸化物粒子が得られる。By the way, regarding the route for obtaining the raw material Fe5Oa, in Japan, a large amount of ferrous sulfate is currently produced as a by-product from Bickling waste liquid or titanium white manufacturing waste liquid, and this V
By appropriately combining reaction conditions from a tfftm-iron solution, the above-mentioned Goethite and black Fe30p iron oxide particles can be obtained.
このような複雑な経路を経て得られる磁性体粉粒子は、
その表面に種々のイオン、例えば、Na” 、 Mn”
、 Cr’◆、 Cr” 、 Ni” 、 Go”
、 SO42−。The magnetic powder particles obtained through such a complicated route are
Various ions such as Na'', Mn'' are present on its surface.
, Cr'◆, Cr", Ni", Go"
, SO42-.
OH−、NO3−、0文−、Br−、I−を残存し、通
常の工業的洗浄では完全に除去されない。OH-, NO3-, 0-, Br-, and I- remain and are not completely removed by normal industrial cleaning.
このような不純物イオンの存在は、高品位で安定した磁
性トナーや磁気テープを得る目的を阻害(しやすい。The presence of such impurity ions tends to impede the purpose of obtaining high-quality and stable magnetic toner or magnetic tape.
たとえば、 Ha 2 SO4”’の存在により、磁
性粉表面が吸湿しやすくなり、製品である磁性トナーや
磁気テープの品質が劣化しやすい。For example, due to the presence of Ha 2 SO 4'', the surface of the magnetic powder tends to absorb moisture, which tends to deteriorate the quality of magnetic toner and magnetic tape products.
また、磁性体は、バインダー(結着剤)と呼ばれる樹脂
中に分散して使用されるところ、表面不純物の存在によ
り樹脂との結合力が弱まりやすく、このために安定した
分散状態の達成、維持が困難になり、したがって、品質
の劣悪化を招来しやすい。In addition, magnetic materials are used dispersed in a resin called a binder, and the presence of surface impurities tends to weaken the bonding force with the resin, resulting in the achievement and maintenance of a stable dispersion state. Therefore, it is easy to cause deterioration in quality.
〔発明が解決しようとする問題点]
本発明は、表面の不純物イオンが除去されるとともに、
表面が親油化処理されてなり、耐湿性や分散性が向上し
た高品質の磁性トナー、磁性インク、磁性塗料、磁気テ
ープなどを与える粉粒状の処理磁性体を提供するために
なされたものである。[Problems to be solved by the invention] In the present invention, impurity ions on the surface are removed, and
This was done in order to provide powder-like treated magnetic material whose surface has been treated to make it oleophilic and which can be used to produce high-quality magnetic toners, magnetic inks, magnetic paints, magnetic tapes, etc., with improved moisture resistance and dispersibility. be.
〔問題点を解決するための手段及び作用]本発明によれ
ば、
(1)表面が脱イオン洗浄処理及び親油化処理されてな
ることを特徴とする粉粒状の処理磁性体、並びに
(2)不純物イオンを含有する粉粒状の磁性体を陽イオ
ン交換樹脂および陰イオン交換樹脂と共に水中に分散し
、撹拌後、水及びイオン交換樹脂を分離し、乾avk、
得られた磁性体の表面に親油化カップリング剤を反応せ
しめることを特徴とする処理磁性体の製造方法
が提供される。[Means and effects for solving the problems] According to the present invention, (1) a powder-like treated magnetic material whose surface is subjected to a deionization cleaning treatment and a lipophilic treatment; ) A powdery magnetic substance containing impurity ions is dispersed in water together with a cation exchange resin and an anion exchange resin, and after stirring, the water and ion exchange resin are separated, and dried AVK,
A method for producing a treated magnetic material is provided, which comprises reacting the surface of the obtained magnetic material with a lipophilic coupling agent.
本発明は、得られた磁性体粉を脱イオン処理し、更にそ
の後に親油化処理することにより構成される。The present invention is constructed by subjecting the obtained magnetic powder to deionization treatment and then further lipophilization treatment.
すなわち、脱イオン処理であるが、磁性体粉をイオン交
換水中に投入し十分に撹拌した後、沈降、遠心か過等に
より水と分離し、このように前洗浄を施した後に、脱イ
オン処理するのが好ましく、脱イオン処理は、イオン交
換水中又は純水中に陽イオン交4!!!!樹脂及び陰イ
オン交換樹脂と共に磁性体粉を投入し、十分に撹拌し、
次いで、水・イオン交換樹脂と分離し、この操作を適当
回数繰返した後、乾燥すればよい。In other words, deionization treatment involves putting magnetic powder into ion-exchanged water, thoroughly stirring it, separating it from the water by sedimentation, centrifugation, filtration, etc., performing pre-cleaning in this way, and then deionization treatment. It is preferable to carry out the deionization treatment by exchanging cations in ion-exchanged water or pure water. ! ! ! Add the magnetic powder together with the resin and anion exchange resin, stir thoroughly,
Next, water and ion exchange resin are separated, and this operation is repeated an appropriate number of times, followed by drying.
本発明に用いるイオン交換樹脂には、陽イオン交換樹脂
、陰イオン交換樹脂があり1例えば三菱化成工業製の「
ダイヤイオン」等がある。Ion exchange resins used in the present invention include cation exchange resins and anion exchange resins.
"Diaion" etc.
本発明に用いる親油化カップリング剤には、具体的商品
名とともに列挙すれば、チタンカップリング剤として市
販されている味の素株式会社製の「フ0レンアクトJ
TTS、 9S、 38S、 418. 46B、
55゜1388、2388などの品種があり、また、日
本曹連株式会社製の「有機チタン製品」のA−1(TP
T)、 B−1(TOT)、 TOT、 TST、 T
AA、 TAT、 TLA、 (Ti蝕C)。The lipophilic coupling agents used in the present invention include "Fuorenact J
TTS, 9S, 38S, 418. 46B,
There are varieties such as 55°1388 and 2388, and there is also A-1 (TP
T), B-1 (TOT), TOT, TST, T
AA, TAT, TLA, (Ti eclipse C).
丁OG、 TBSTA、 A−10・(TPT ポリマ
ー)、 B−2,B−4゜B−7,B−10(以上TB
Tポリマー)、 TBSTA−400(TBSTAポリ
マー)、 TTS、 TOA−30,TSDMA、 T
TAB。Ding OG, TBSTA, A-10・(TPT polymer), B-2, B-4゜B-7, B-10 (more than TB
T polymer), TBSTA-400 (TBSTA polymer), TTS, TOA-30, TSDMA, T
T.A.B.
TTOPなどがあり、また市販のシランカップリング剤
も用いることができる。Examples include TTOP, and commercially available silane coupling agents can also be used.
本発明に用いる磁性体は市販のいずれもが適用可能であ
り、例えば戸田工業製のrMAT 120 JrMAT
210 J rEPT 500 J rMAT
115 J rEPTloooJ 、三井金属工業製
のrMG−W」、東京電気化学工業型のrcAP−I
J rcAP−2J等すべてが用いることができる。Any commercially available magnetic material can be used as the magnetic material used in the present invention, such as rMAT 120 JrMAT manufactured by Toda Kogyo.
210 J rEPT 500 J rMAT
115 J rEPTloooJ, rMG-W manufactured by Mitsui Kinzoku Kogyo, Tokyo Denki Kagaku Kogyo type rcAP-I
JrcAP-2J etc. can all be used.
[実施例] 次に実施例を挙げて本発明を説明する。[Example] Next, the present invention will be explained with reference to Examples.
実施例1
磁性体として戸田工業製rMAT 210 J 10k
gをイオン交換水(電導率0.2μ5)50交中へ投入
し20分間撹拌した。この上澄液の主導率は85μsで
あった0次に、ト澄液を除去し、更に50交の上記イオ
ン交換水を投入し同様に撹拌すると、上澄液の溶出電導
−(には40g5に低ドした。そこで1次に見掛量32
の「ダイヤイオンSA l0AJ (三菱化成工業製
)と同字の「ダイヤイオン5KIBJ(三菱化成工業f
M)とを合わせ投入し60分撹拌したところ、溶出電導
率は8gSであった。このように脱イオン処理した磁性
体を分離し、次いで乾燥し、脱イオン処理磁性体を得た
。Example 1 Toda Kogyo rMAT 210 J 10k as magnetic material
g was added to 50 g of ion-exchanged water (electrical conductivity: 0.2μ5) and stirred for 20 minutes. The conductivity of this supernatant liquid was 85 μs.Next, the supernatant liquid was removed, and the above ion-exchanged water was added and stirred in the same manner. Therefore, the primary apparent amount is 32
"Diaion SA 10AJ (manufactured by Mitsubishi Chemical Industries) and "Diaion 5KIBJ (manufactured by Mitsubishi Chemical Industries, Ltd.)"
When the mixture was mixed with M) and stirred for 60 minutes, the elution conductivity was 8 gS. The deionized magnetic material was separated and then dried to obtain a deionized magnetic material.
この脱イオン処理磁性体を更に親油化処理した。乾燥し
た脱イオン磁性体3kgに「プレンアクトTTS J
45gを加えミキサーにて十分撹拌し、発1 生ずる
イソプロピルアルコールを除去した。This deionized magnetic material was further subjected to lipophilic treatment. 3 kg of dry deionized magnetic material
45 g was added and sufficiently stirred with a mixer to remove the isopropyl alcohol produced.
このように処理した本発明の磁性体60重量部に対し、
ポリスチレン:ピコアスチックD−125(エンソスタ
ンダード石油) 90ffif1部ポリプロピレン:
860P (三洋化成) 10重量部を配合して熱ロー
ルミルにより150°Cで1時間混練後、冷却し、カッ
ターミルで粗粉砕してからジェットミルを使って微粉砕
し、1〜30給のトナー微粒子を得た。For 60 parts by weight of the magnetic material of the present invention treated in this way,
Polystyrene: Pico-Stick D-125 (Enso Standard Oil) 90ffif 1 part Polypropylene:
860P (Sanyo Kasei) 10 parts by weight was blended and kneaded for 1 hour at 150°C with a hot roll mill, cooled, coarsely ground with a cutter mill, and then finely ground with a jet mill to produce toner of 1 to 30 parts. Fine particles were obtained.
上記トナーを風力分級器を用い5〜20牌の粒子を?’
)だ、そのときの体積平均粒径は14pmであった。Using a wind classifier to separate the above toner into particles of 5 to 20 tiles? '
), the volume average particle diameter at that time was 14 pm.
上記本発明の処理磁性体を用いて調整した一成分磁性ト
ナーを、未処理の磁性体及び脱イオン処理のみ施した磁
性体を用いて調整したトナーと比較した。A one-component magnetic toner prepared using the above-mentioned treated magnetic material of the present invention was compared with toner prepared using an untreated magnetic material and a magnetic material subjected to only deionization treatment.
本発明及び脱イオン処理品においては良好な粒度を得た
が、一方、未処理品においては粗い粒度となり、分級に
より、体積平均径をt4g曹に合わせた。Good particle size was obtained in the present invention and the deionized product, but on the other hand, in the untreated product, the particle size was coarse, and the volume average diameter was adjusted to t4g soda by classification.
更に比較のため、トナーの吸湿率を測定した。Furthermore, for comparison, the moisture absorption rate of the toner was measured.
吸湿率は、25℃における水と共にデシケータに密封す
るトナーの重量増加により求めたところ、処理磁性体に
よるトナーでは24時間で0.2%であったのに対し、
脱イオンのみの磁性体によるトナーでは0.3%、未処
理のでは0.6%であった。The moisture absorption rate was determined by increasing the weight of the toner sealed in a desiccator with water at 25°C, and it was 0.2% in 24 hours for the toner made of treated magnetic material.
It was 0.3% for toner made of magnetic material that was only deionized, and 0.6% for untreated toner.
更・にトナーの耐湿性を複写機による実焼耐久試験を行
ない比較した。キャノン製の電子写真式の複写機PC−
20を用い、温度35℃、湿度85%RHの高温高湿下
におけるテストを行なったところ、耐久枚数2,000
枚における最大画像濃度が未処理磁性体によるトナーで
は0.35まで、脱イオン処理した磁性体によるトナー
では0.55まで各々低下したのに対し、脱イオン処理
後親油化処理した磁性体によるトナーでは0.85とい
う高い値を維持した。Furthermore, the moisture resistance of the toner was compared by conducting an actual firing durability test using a copying machine. Canon electrophotographic copying machine PC-
20 was tested at a high temperature and high humidity of 35℃ and 85% RH, and the durability was 2,000 sheets.
The maximum image density on the sheet decreased to 0.35 with the toner made of untreated magnetic material and to 0.55 with the toner made with deionized magnetic material, whereas The toner maintained a high value of 0.85.
[発明の効果]
本発明の磁性体は上記のように、表面が脱イオン洗浄処
理及び親油化処理されていて、吸湿性を与え磁性体表面
と樹脂との結合力を弱めていた不純物イオンが除去され
、しかも親油化処理されていて樹脂との親和性が良いた
めに、耐湿性や分散性が向上した高品質の磁性トナー、
磁性インク。[Effects of the Invention] As described above, the surface of the magnetic body of the present invention has been subjected to deionization cleaning treatment and lipophilization treatment, and the impurity ions that impart hygroscopicity and weaken the bonding force between the magnetic body surface and the resin are removed. This is a high-quality magnetic toner with improved moisture resistance and dispersibility, as it has been treated to be lipophilic and has good affinity with resin.
magnetic ink.
磁性w p+ 、磁気テープなどを与え得るものである
。また、本発明の製造方法においては、上記の物性に優
れた処理磁性体を容易に得ることができる。Magnetic w p+ , magnetic tape, etc. can be provided. Further, in the manufacturing method of the present invention, a treated magnetic material having excellent physical properties as described above can be easily obtained.
Claims (2)
ることを特徴とする粉粒状の処理磁性体。(1) A powder-like treated magnetic material whose surface has been subjected to deionization cleaning treatment and lipophilic treatment.
ン交換樹脂および陰イオン交換樹脂と共に水中に分散し
、撹拌後、水及びイオン交換樹脂を分離し、乾燥後、得
られた磁性体の表面に親油化カップリング剤を反応せし
めることを特徴とする処理磁性体の製造方法。(2) A powdery magnetic material containing impurity ions is dispersed in water together with a cation exchange resin and an anion exchange resin, and after stirring, the water and ion exchange resin are separated, and after drying, the obtained magnetic material is A method for producing a treated magnetic material, characterized by reacting a lipophilic coupling agent on the surface.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP59224129A JPS61102706A (en) | 1984-10-26 | 1984-10-26 | Magnetic material to be treated and manufacture thereof |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP59224129A JPS61102706A (en) | 1984-10-26 | 1984-10-26 | Magnetic material to be treated and manufacture thereof |
Publications (1)
Publication Number | Publication Date |
---|---|
JPS61102706A true JPS61102706A (en) | 1986-05-21 |
Family
ID=16808993
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP59224129A Pending JPS61102706A (en) | 1984-10-26 | 1984-10-26 | Magnetic material to be treated and manufacture thereof |
Country Status (1)
Country | Link |
---|---|
JP (1) | JPS61102706A (en) |
-
1984
- 1984-10-26 JP JP59224129A patent/JPS61102706A/en active Pending
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