JPH0665201B2 - Magnetic fluid manufacturing method - Google Patents
Magnetic fluid manufacturing methodInfo
- Publication number
- JPH0665201B2 JPH0665201B2 JP19432284A JP19432284A JPH0665201B2 JP H0665201 B2 JPH0665201 B2 JP H0665201B2 JP 19432284 A JP19432284 A JP 19432284A JP 19432284 A JP19432284 A JP 19432284A JP H0665201 B2 JPH0665201 B2 JP H0665201B2
- Authority
- JP
- Japan
- Prior art keywords
- magnetic fluid
- dicarboxylic acid
- producing
- fine particles
- solvent
- 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 - Lifetime
Links
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/44—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of magnetic liquids, e.g. ferrofluids
- H01F1/442—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of magnetic liquids, e.g. ferrofluids the magnetic component being a metal or alloy, e.g. Fe
Description
【発明の詳細な説明】 Ｉ 発明の背景 技術分野 本発明は、磁性流体の製造方法に関する。Description: BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing magnetic fluid.
先行技術とその問題点 磁性流体としては、既に、酸化物磁性材料（マグネタイ
ト、Fe３Ｏ４）の微粒子を表面活性剤で処理して、油
類、水等の中にコロイド状に分散させたものが知られて
おり、実際、多岐の分野で実用化されている。Prior art and its problems As a magnetic fluid, fine particles of an oxide magnetic material (magnetite, Fe 3 O 4 ) have already been treated with a surfactant and dispersed in oils, water, etc. in a colloidal state. Things are known and are actually put to practical use in various fields.
例えば、回転軸シール等の各種シールへの応用が一般的
に知られている。For example, application to various seals such as a rotary shaft seal is generally known.
これらの応用用途において、実用上、溶媒の低揮発性、
熱安定性、潤滑性等が要求されることが多い。In these applications, practically low solvent volatility,
Thermal stability and lubricity are often required.
このような要件を満たす溶媒として、脂肪酸のエステル
もしくはジエステル系、ポリフェニル油系等が好適であ
ることが知られており、酸化物磁性流体では、これらの
溶媒を使用した磁性流体が既に作製されている。It is known that esters or diesters of fatty acids, polyphenyl oils, and the like are suitable as a solvent satisfying such requirements, and in the magnetic fluid of oxides, magnetic fluids using these solvents have already been prepared. ing.
しかし、分散微粒子そのものの飽和磁化の高い金属微粒
子を用いては、まだ、成功していない。金属微粒子を用
いて、上記の溶媒を使用した金属微粒子の濃度の高い磁
性流体の作製が可能ならば、飽和磁化が高くかつ熱安定
性等に優れた磁性流体を得ることができ、更に応用範囲
が広がることが期待される。However, the use of metallic fine particles having high saturation magnetization of dispersed fine particles itself has not been successful yet. If it is possible to produce a magnetic fluid having a high concentration of the metal fine particles using the above-mentioned solvent using the metal fine particles, it is possible to obtain a magnetic fluid having a high saturation magnetization and excellent thermal stability, and the range of application. Is expected to spread.
II 発明の目的 本発明の目的は、一般的でかつ比較的安価な原料である
鉄を使用して、その金属微粒子を高沸点溶媒に分散さ
せ、従来の磁性流体に比べて高い飽和磁化を有し、かつ
実用的な磁性流体の製造方法を得ることにある。II Object of the Invention The object of the present invention is to use iron, which is a general and relatively inexpensive raw material, to disperse its metal fine particles in a high-boiling point solvent and to have a saturation magnetization higher than that of a conventional magnetic fluid. And to obtain a practical magnetic fluid manufacturing method.
このような目的は、下記の本発明によって達成される。Such an object is achieved by the present invention described below.
すなわち、本発明は、鉄の金属微粒子と、界面活性剤
と、ジカルボン酸ジエステル系の溶媒とを含む磁性流体
を得るに際し、 鉄のカルボニル化合物と、前記界面活性剤と、前記溶媒
とを含む溶液を加熱する磁性流体の製造方法である。That is, the present invention, when obtaining a magnetic fluid containing iron metal fine particles, a surfactant, and a dicarboxylic acid diester-based solvent, a solution containing an iron carbonyl compound, the surfactant, and the solvent It is a method for producing a magnetic fluid for heating a magnetic field.
III 発明の具体的構成 以下、本発明の具体的構成について詳細に説明する。III Specific Structure of the Invention Hereinafter, the specific structure of the present invention will be described in detail.
本発明の鉄の金属微粒子を用いた磁性流体では、まず、
強磁性微粒子を液体中で分散させることが不可欠である
ため、その磁気的凝集力に打ち勝つような粒径にする必
要かある。In the magnetic fluid using the iron metal fine particles of the present invention, first,
Since it is essential to disperse the ferromagnetic fine particles in the liquid, it is necessary to make the particle size so as to overcome the magnetic cohesive force.
本発明では、鉄金属微粒子は70〜100Åのものを用い
る。In the present invention, fine iron metal particles having a particle size of 70 to 100 liters are used.
磁性流体には、溶媒の低揮発性、熱安定性、潤滑性等が
要求されるために、本発明では溶媒としてジカルボン酸
ジエステル系の溶媒を用いる。Since the magnetic fluid is required to have low volatility, thermal stability, lubricity and the like of the solvent, a dicarboxylic acid diester-based solvent is used as the solvent in the present invention.
ジカルボン酸ジエステルは、炭素原子数６〜10の脂肪族
飽和ジカルボン酸のジエステルであることが好ましく、
下記式〔Ｉ〕で示される。The dicarboxylic acid diester is preferably a diester of an aliphatic saturated dicarboxylic acid having 6 to 10 carbon atoms,
It is represented by the following formula [I].
ROOC（CH２）nCOOR 上記式〔Ｉ〕において、ｎ＝４〜８であり、脂肪族飽和
ジカルボン酸としては、ｎ＝４のアジピン酸、ｎ＝７の
アゼライン酸、ｎ＝８のセバシン酸等が好ましい。ROOC (CH 2 ) nCOOR In the above formula [I], n = 4 to 8, and as the aliphatic saturated dicarboxylic acid, adipic acid with n = 4, azelaic acid with n = 7, sebacic acid with n = 8, etc. Is preferred.
Ｒは、脂肪族飽和炭化水素基であり、炭素原子数１〜10
のもの、特にオクチル基であることが好ましい。R is an aliphatic saturated hydrocarbon group having 1 to 10 carbon atoms
And particularly preferably an octyl group.
すなわち、好適に用いられる溶媒は、上記の脂肪族飽和
ジカルボン酸とオクチルアルコール（１−オクタノール
または２−エチルヘキシルアルコール）とのエステル化
物であり、下記のものをあげることができる。That is, the solvent preferably used is an esterified product of the above aliphatic saturated dicarboxylic acid and octyl alcohol (1-octanol or 2-ethylhexyl alcohol), and the following can be mentioned.
ｉ）アジピン酸ジ（２−エチルヘキシル） ii）アゼライン酸ジ（２−エチルヘキシル） iii）セバシン酸ジ（２−エチルヘキシル） これらは混合して用いてもよい。i) di (2-ethylhexyl) adipate ii) di (2-ethylhexyl) azelate iii) di (2-ethylhexyl) sebacate These may be used as a mixture.
これらのジカルボン酸ジエステル系溶媒は、金属微粒子
に対して100〜800重量％含まれる。These dicarboxylic acid diester solvents are contained in an amount of 100 to 800% by weight based on the metal fine particles.
一方、ファンデルワールスの引力による凝集を防ぐた
め、酸化物磁性粒子の場合、極性分子の界面活性剤を用
いて化学的にコーティングして、粒子同志の反発による
凝集を防いでいる。On the other hand, in order to prevent aggregation due to van der Waals attraction, oxide magnetic particles are chemically coated with a surfactant of polar molecules to prevent aggregation due to repulsion between the particles.
しかし、金属磁性流体の場合、この種のコーティング剤
は見い出されていなかった。However, no coating agent of this kind has been found in the case of metallic magnetic fluid.
本発明では、界面活性剤としてリン脂質を用いることが
好ましい。In the present invention, it is preferable to use phospholipid as the surfactant.
すなわち、この場合、用いるリン脂質はレシチンであ
り、大豆により得られた天然のもの、あるいはこれを精
製したもののいずれであってもよい。That is, in this case, the phospholipid used is lecithin, which may be a natural one obtained from soybean or a purified one.
レシチンは、下記式〔II〕で示される。Lecithin is represented by the following formula [II].
〔II〕レシチン（ホスファチジルコリン） 上記式〔II〕において、Ｒ１およびＲ２は飽和または不
飽和脂肪酸である。すなわち、パルミチン酸、ステアリ
ン酸、オレイン酸、リノール酸、リノレン酸等、炭素原
子数20程度以下のものである。[II] Lecithin (phosphatidylcholine) In the above formula [II], R 1 and R 2 are saturated or unsaturated fatty acids. That is, palmitic acid, stearic acid, oleic acid, linoleic acid, linolenic acid and the like having about 20 or less carbon atoms.
なお、Ｒ１とＲ２は、異なっていても、同じであっても
よい。Note that R 1 and R 2 may be different or the same.
添加する界面活性剤は、金属微粒子に対して50〜100重
量％程度である。The surfactant added is about 50 to 100% by weight with respect to the metal fine particles.
50重量％未満では実効がなく、100重量％を越えると、
凝集してしまい分散しない。If it is less than 50% by weight, it is not effective, and if it exceeds 100% by weight,
It does not disperse because it aggregates.
なお、レシチンは、市販のものを用いればよい。As lecithin, a commercially available product may be used.
このような磁性流体を作製するには、界面活性剤を溶解
させたジカルボン酸ジエステル系溶媒中に金属カルボニ
ルを加え、混合溶液を加熱し、金属カルボニルの熱分解
を行えばよい。To prepare such a magnetic fluid, metal carbonyl may be added to a dicarboxylic acid diester solvent in which a surfactant is dissolved, and the mixed solution may be heated to thermally decompose the metal carbonyl.
金属カルボニルとしてはFe（CO）５を用いればよい。Fe (CO) 5 may be used as the metal carbonyl.
また、熱分解温度は140〜280℃、熱分解時間は４〜６時
間程度とする。温度および時間については、鉄の濃度に
よって適宜変更すればよい。The thermal decomposition temperature is 140 to 280 ° C, and the thermal decomposition time is 4 to 6 hours. The temperature and time may be appropriately changed depending on the iron concentration.
このような磁性流体は、所定の容器に入れておく必要が
ある。そして、容器内はアルゴン窒素等の不活性ガスで
置換することが好ましい。Such a magnetic fluid needs to be stored in a predetermined container. Then, it is preferable to replace the inside of the container with an inert gas such as argon nitrogen.
IV 発明の具体的作用効果 本発明によって得られる磁性流体は、飽和磁化の高いFe
の金属微粒子を用いており、かつ、界面活性剤にリン脂
質を用いて高沸点溶媒であるジカルボン酸ジエステル系
媒体中に金属微粒子を分散させているため、分散性にす
ぐれ、従来の磁性流体に比べ高い飽和磁化を有するもの
である。IV Specific Actions and Effects of the Invention The magnetic fluid obtained by the present invention is Fe with high saturation magnetization.
The fine metal particles are used, and the fine metal particles are dispersed in the dicarboxylic acid diester medium, which is a high-boiling-point solvent, using phospholipids as the surfactant. It has a higher saturation magnetization than that.
また、媒体中にジカルボン酸ジエステル系媒体を用いて
いるため、溶媒の低揮発性、熱安定性、潤滑性等が満足
され、実用上有利である。Further, since the dicarboxylic acid diester-based medium is used in the medium, low volatility, thermal stability, lubricity and the like of the solvent are satisfied, which is practically advantageous.
さらに、金属微粒子にFeを用いているので、Coを用いた
場合に比べてコストの低減がはかられる。Further, since Fe is used for the metal fine particles, the cost can be reduced as compared with the case where Co is used.
Ｖ 発明の具体的実施例 以下、本発明の具体的実施例を示し、本発明をさらに詳
細に説明する。V Specific Examples of the Invention Hereinafter, specific examples of the present invention will be shown to explain the present invention in more detail.
＜実施例１＞ レシチン4gをアジピン酸ジオクチル12gに溶解させた溶
液を、冷却器、温度計、撹拌装置をつけた３つの口フラ
スコに入れた。これにペンタカルボニル鉄Fe（CO）５8g
を加えた。<Example 1> A solution prepared by dissolving 4 g of lecithin in 12 g of dioctyl adipate was placed in a three-necked flask equipped with a condenser, a thermometer, and a stirrer. This iron pentacarbonyl Fe (CO) 5 8g
Was added.
この混合溶液を撹拌しながら、マントルヒーターで徐々
に加熱し、還流を行いながら鉄カルボニルの熱分解を行
った。この際、冷却器上部から分解してできたCOが発生
する。このCOの発生はPdCl２溶液（アセトン：水＝1:
1）に通すことによって確認した。This mixed solution was gradually heated with a mantle heater while stirring, and the pyrolysis of iron carbonyl was performed while refluxing. At this time, CO generated by decomposition from the upper part of the cooler is generated. This generation of CO occurs in a PdCl 2 solution (acetone: water = 1: 1).
Confirmed by passing through 1).
すなわち、橙色のPdCl２溶液はCOの導入により黒色に変
化するからである。That is, the orange PdCl 2 solution turns black by the introduction of CO.
COの発生が終了してから、約30分間撹拌を続けた後、冷
却した。これにより、黒色の溶液ができた。この黒色の
溶液を6000rpmの遠心下で１時間遠心分離を行った。After the generation of CO was completed, stirring was continued for about 30 minutes and then cooled. This produced a black solution. This black solution was centrifuged at 6000 rpm for 1 hour.
しかしこの時、ほとんど分離沈降はなかった。However, at this time, there was almost no separation and sedimentation.
アジピン酸ジオクチルの量を変化させることにより、磁
性流体の濃度を変化させることが可能である。By changing the amount of dioctyl adipate it is possible to change the concentration of the magnetic fluid.
得られた溶液の比重と飽和磁化の関係を表１および第１
図に示す（ここでは、濃度の代りに比重をパラメータに
した）。The relationship between the specific gravity and the saturation magnetization of the obtained solution is shown in Table 1 and Table 1.
It is shown in the figure (here, specific gravity is used as a parameter instead of concentration).
＜実施例２＞ 実施例１にて、アジピン酸ジオクチルの代りに、溶媒と
してセバチン酸ジオクチルを使った。得られた黒色の溶
液を6000rpmの遠心下で10時間遠心分離を行ったが、ほ
とんど分離沈降はなかった。 <Example 2> In Example 1, dioctyl sebacate was used as a solvent instead of dioctyl adipate. The obtained black solution was centrifuged at 6000 rpm for 10 hours, but almost no sedimentation occurred.
溶液の比重1.4251で、飽和磁化は500Gであった。The specific gravity of the solution was 1.4251, and the saturation magnetization was 500G.
＜実施例３＞ 実施例１でアジピン酸ジオクチルの代りに溶媒としてア
ゼラチン酸ジ（２−エチルヘキシル）を使った。<Example 3> In Example 1, di (2-ethylhexyl) agelate was used as a solvent instead of dioctyl adipate.
溶液の比重1.3612で、飽和磁化は312Gであった。The specific gravity of the solution was 1.3612, and the saturation magnetization was 312G.
以上より、本発明の効果は明らかである。From the above, the effect of the present invention is clear.
第１図は、高沸点溶媒にアジピン酸ジオクチルを使っ
て、界面活性剤として、レシチンを用いた時の鉄磁性流
体の比重と飽和磁化（４πMs／Ｇ）との関係を示すグラ
フである。FIG. 1 is a graph showing the relationship between the specific gravity of iron magnetic fluid and the saturation magnetization (4πMs / G) when dioctyl adipate was used as the high boiling point solvent and lecithin was used as the surfactant.
───────────────────────────────────────────────────── フロントページの続き (51)Int.Cl.5 識別記号 庁内整理番号 ＦＩ 技術表示箇所 Ｃ１０Ｎ 20:06 Ｚ 8217−4Ｈ 30:04 8217−4Ｈ 30:06 8217−4Ｈ 30:08 8217−4Ｈ 40:14 8217−4Ｈ ─────────────────────────────────────────────────── ─── Continuation of the front page (51) Int.Cl. 5 Identification code Office reference number FI Technical display location C10N 20:06 Z 8217-4H 30:04 8217-4H 30:06 8217-4H 30:08 8217- 4H 40:14 8217-4H
Claims (8)
ボン酸ジエステル系の溶媒とを含む磁性流体を得るに際
し、 鉄のカルボニル化合物と、前記界面活性剤と、前記溶媒
とを含む溶液を加熱する磁性流体の製造方法。1. When obtaining a magnetic fluid containing iron metal fine particles, a surfactant, and a dicarboxylic acid diester-based solvent, a solution containing an iron carbonyl compound, the surfactant, and the solvent is used. A method for producing a magnetic fluid to be heated.
る特許請求の範囲第１項の磁性流体の製造方法。2. The method for producing a magnetic fluid according to claim 1, wherein the average particle system of the metal fine particles is 70 to 100Å.
原子数６〜10の脂肪族飽和ジカルボン酸のジエステルで
ある特許請求の範囲第１項または第２項の磁性流体の製
造方法。3. The method for producing a magnetic fluid according to claim 1 or 2, wherein the dicarboxylic acid diester-based solvent is a diester of an aliphatic saturated dicarboxylic acid having 6 to 10 carbon atoms.
ルボン酸と炭素原子数１〜10の脂肪族アルコールとのエ
ステル化物である特許請求の範囲第１項ないし第３項の
いずれかの磁性流体の製造方法。4. The magnetic fluid according to any one of claims 1 to 3, wherein the dicarboxylic acid diester solvent is an esterified product of dicarboxylic acid and an aliphatic alcohol having 1 to 10 carbon atoms. Production method.
微粒子に対し、100〜800重量％含有される特許請求の範
囲第１項ないし第４項のいずれかの磁性流体の製造方
法。5. The method for producing a magnetic fluid according to any one of claims 1 to 4, wherein the dicarboxylic acid diester-based solvent is contained in an amount of 100 to 800% by weight based on the metal fine particles.
囲第１項ないし第５項のいずれかの磁性流体の製造方
法。6. The method for producing a magnetic fluid according to any one of claims 1 to 5, wherein the surfactant is a phospholipid.
囲第１項ないし第６項のいずれかの磁性流体の製造方
法。7. The method for producing a magnetic fluid according to any one of claims 1 to 6, wherein the phospholipid is lecithin.
重量％含有される特許請求の範囲第１項ないし第７項の
いずれかの磁性流体の製造方法。8. The surfactant is 50-100 with respect to the metal fine particles.
The method for producing a magnetic fluid according to any one of claims 1 to 7, wherein the magnetic fluid is contained in a weight percentage.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP19432284A JPH0665201B2 (en) | 1984-09-17 | 1984-09-17 | Magnetic fluid manufacturing method |
| US06/775,356 US4626370A (en) | 1984-09-17 | 1985-09-12 | Magnetic fluid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP19432284A JPH0665201B2 (en) | 1984-09-17 | 1984-09-17 | Magnetic fluid manufacturing method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS6171604A JPS6171604A (en) | 1986-04-12 |
| JPH0665201B2 true JPH0665201B2 (en) | 1994-08-22 |
Family
ID=16322663
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP19432284A Expired - Lifetime JPH0665201B2 (en) | 1984-09-17 | 1984-09-17 | Magnetic fluid manufacturing method |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0665201B2 (en) |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS58174495A (en) * | 1982-04-07 | 1983-10-13 | Nippon Seiko Kk | Preparation of magnetic fluid |
-
1984
- 1984-09-17 JP JP19432284A patent/JPH0665201B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPS6171604A (en) | 1986-04-12 |
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