JPH02239603A - Magnetic fluid composition - Google Patents
Magnetic fluid compositionInfo
- Publication number
- JPH02239603A JPH02239603A JP6127489A JP6127489A JPH02239603A JP H02239603 A JPH02239603 A JP H02239603A JP 6127489 A JP6127489 A JP 6127489A JP 6127489 A JP6127489 A JP 6127489A JP H02239603 A JPH02239603 A JP H02239603A
- Authority
- JP
- Japan
- Prior art keywords
- magnetic fluid
- solvent
- carbonyl
- group
- fine particles
- 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
- 239000011553 magnetic fluid Substances 0.000 title claims abstract description 30
- 239000000203 mixture Substances 0.000 title claims abstract description 21
- 239000002904 solvent Substances 0.000 claims abstract description 19
- 229910017052 cobalt Inorganic materials 0.000 claims abstract description 17
- 239000010941 cobalt Substances 0.000 claims abstract description 17
- 239000002270 dispersing agent Substances 0.000 claims abstract description 14
- 125000000217 alkyl group Chemical group 0.000 claims abstract description 10
- WGQKYBSKWIADBV-UHFFFAOYSA-N benzylamine Chemical compound NCC1=CC=CC=C1 WGQKYBSKWIADBV-UHFFFAOYSA-N 0.000 claims abstract description 10
- 125000003342 alkenyl group Chemical group 0.000 claims abstract description 6
- -1 alkenyl succinic imide Chemical compound 0.000 claims abstract description 5
- 229940087654 iron carbonyl Drugs 0.000 claims abstract description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 17
- 239000010419 fine particle Substances 0.000 claims description 17
- 229910052751 metal Inorganic materials 0.000 claims description 14
- 239000002184 metal Substances 0.000 claims description 14
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 12
- 125000004432 carbon atom Chemical group C* 0.000 claims description 9
- 229910052742 iron Inorganic materials 0.000 claims description 9
- 229910001111 Fine metal Inorganic materials 0.000 claims description 4
- 239000002923 metal particle Substances 0.000 claims description 4
- 125000001931 aliphatic group Chemical group 0.000 claims description 3
- 239000000696 magnetic material Substances 0.000 claims description 2
- 239000000126 substance Substances 0.000 claims 3
- 239000012530 fluid Substances 0.000 claims 1
- 230000005415 magnetization Effects 0.000 abstract description 24
- 238000000034 method Methods 0.000 abstract description 10
- 229960002317 succinimide Drugs 0.000 abstract description 4
- 229920006395 saturated elastomer Polymers 0.000 abstract description 2
- 239000013528 metallic particle Substances 0.000 abstract 2
- 125000001183 hydrocarbyl group Chemical group 0.000 abstract 1
- 239000002244 precipitate Substances 0.000 abstract 1
- 239000003350 kerosene Substances 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 229920000768 polyamine Polymers 0.000 description 6
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 5
- 239000006185 dispersion Substances 0.000 description 4
- 125000000816 ethylene group Chemical group [H]C([H])([*:1])C([H])([H])[*:2] 0.000 description 4
- 239000004094 surface-active agent Substances 0.000 description 4
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- KZNICNPSHKQLFF-UHFFFAOYSA-N dihydromaleimide Natural products O=C1CCC(=O)N1 KZNICNPSHKQLFF-UHFFFAOYSA-N 0.000 description 3
- 229930195733 hydrocarbon Natural products 0.000 description 3
- 150000002430 hydrocarbons Chemical class 0.000 description 3
- 239000002480 mineral oil Substances 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 2
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 2
- 229910002091 carbon monoxide Inorganic materials 0.000 description 2
- 150000004985 diamines Chemical class 0.000 description 2
- 238000001879 gelation Methods 0.000 description 2
- 150000003949 imides Chemical class 0.000 description 2
- 235000010446 mineral oil Nutrition 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 229920001281 polyalkylene Polymers 0.000 description 2
- 229920013639 polyalphaolefin Polymers 0.000 description 2
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 2
- 238000004062 sedimentation Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 238000005979 thermal decomposition reaction Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229910001868 water Inorganic materials 0.000 description 2
- IIZPXYDJLKNOIY-JXPKJXOSSA-N 1-palmitoyl-2-arachidonoyl-sn-glycero-3-phosphocholine Chemical compound CCCCCCCCCCCCCCCC(=O)OC[C@H](COP([O-])(=O)OCC[N+](C)(C)C)OC(=O)CCC\C=C/C\C=C/C\C=C/C\C=C/CCCCC IIZPXYDJLKNOIY-JXPKJXOSSA-N 0.000 description 1
- VILCJCGEZXAXTO-UHFFFAOYSA-N 2,2,2-tetramine Chemical compound NCCNCCNCCN VILCJCGEZXAXTO-UHFFFAOYSA-N 0.000 description 1
- FALRKNHUBBKYCC-UHFFFAOYSA-N 2-(chloromethyl)pyridine-3-carbonitrile Chemical compound ClCC1=NC=CC=C1C#N FALRKNHUBBKYCC-UHFFFAOYSA-N 0.000 description 1
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 235000017788 Cydonia oblonga Nutrition 0.000 description 1
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 description 1
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 1
- 238000006683 Mannich reaction Methods 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000011554 ferrofluid Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000000787 lecithin Substances 0.000 description 1
- 229940067606 lecithin Drugs 0.000 description 1
- 235000010445 lecithin Nutrition 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 239000012188 paraffin wax Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- WTJKGGKOPKCXLL-RRHRGVEJSA-N phosphatidylcholine Chemical compound CCCCCCCCCCCCCCCC(=O)OC[C@H](COP([O-])(=O)OCC[N+](C)(C)C)OC(=O)CCCCCCCC=CCCCCCCCC WTJKGGKOPKCXLL-RRHRGVEJSA-N 0.000 description 1
- 150000003904 phospholipids Chemical class 0.000 description 1
- 229920001083 polybutene Polymers 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- KIDHWZJUCRJVML-UHFFFAOYSA-N putrescine Chemical compound NCCCCN KIDHWZJUCRJVML-UHFFFAOYSA-N 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229940014800 succinic anhydride Drugs 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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
Landscapes
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Lubricants (AREA)
- Soft 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Ａ体組成物に関する。さらに詳細には、
本発明は、特定の分散剤と特定の方法で製造されたコバ
ルトあるいは鉄の金属微粒子を含有することで特徴づけ
られる高磁化を有しかつ安定な磁性流体組成物に関する
ものである。DETAILED DESCRIPTION OF THE INVENTION (Industrial Application Field) The present invention relates to a magnetic A-body composition. In more detail,
The present invention relates to a highly magnetized and stable magnetic fluid composition characterized by containing a specific dispersant and fine metal particles of cobalt or iron produced by a specific method.
磁性流体は磁性微粒子に界面活性剤を吸着させ、水、ケ
ロンン、鉱油等の各種溶媒に分散させてなるコロイド懸
濁液であり、重力、遠心力、磁場等の作用下においても
固・液分離の生じない非常に安定な磁気感能性の液体で
あり、回転シール、比重選別、インクジェットプリンタ
ー、ディスプレイおよび各種センサー等の産業分野の多
方面への利用が期待されている。A magnetic fluid is a colloidal suspension made by adsorbing a surfactant onto magnetic fine particles and dispersing it in various solvents such as water, chlorine, and mineral oil. It is an extremely stable magnetically sensitive liquid that does not generate any turbulence, and is expected to be used in a variety of industrial fields such as rotary seals, specific gravity sorting, inkjet printers, displays, and various sensors.
（従来の技術）
磁性流体としては、既に、酸化物磁性材料（マグネタイ
ト、ＦｅｓＯ４）の微粒子を界面活性剤で処理し、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) Magnetic fluids are already known in which fine particles of oxide magnetic materials (magnetite, FesO4) are treated with a surfactant and dispersed in colloidal form in oil, water, etc. It has actually been put into practical use in a wide variety of fields.
しかし、マグネタイト等を使用する限り、磁性流体とし
ての飽和磁化が２００〜３００ガウス、最高のものでも
５５０〜６００ガウスのものしか得られていないため、
さらに高磁化に応用する場合、飽和磁化が小さいことが
大きな欠点となっている。However, as long as magnetite etc. are used, the saturation magnetization as a magnetic fluid is only 200 to 300 Gauss, and the best one is only 550 to 600 Gauss.
Furthermore, when applied to high magnetization, the small saturation magnetization is a major drawback.
この飽和磁化を高めるためには、分散微粒子そのものの
飽和磁化を高めるか、溶媒中の微粒子の含有量を大きく
するかの２方法がある。There are two methods for increasing this saturation magnetization: increasing the saturation magnetization of the dispersed fine particles themselves, or increasing the content of fine particles in the solvent.
後者の微粒子の濃度をあげる方法としては、特願昭６３
−８２０５３等に記載されたものがあるが、磁性流体が
ペースト状になるなどの問題があるため、マグネタイト
を用いた場合には６００ガウス以上のものを得るのは不
可能である。The latter method of increasing the concentration of fine particles is described in Japanese Patent Application No. 63.
-82053, etc., but due to problems such as the magnetic fluid becoming paste-like, it is impossible to obtain a magnetic field of 600 Gauss or more when magnetite is used.
前者の飽和磁化の高い微粒子を用いた磁性流体としては
、米国特許第３，２２８，８８１号および第３．２２８
，８８２号に記載されているものがある。すなわち、コ
バルトカルボニルＣｏｔ（Ｃｏ）ｓあるいは鉄カルボニ
ルｒｅ（Ｃｏ）ｓをスチレンとアクリロニトリルの共重
体中で熱分解し、炭化水素媒体中に分散させる方法であ
る。The former magnetic fluid using fine particles with high saturation magnetization is disclosed in U.S. Pat. Nos. 3,228,881 and 3.228.
, No. 882. That is, this is a method in which cobalt carbonyl Cot(Co)s or iron carbonyl re(Co)s is thermally decomposed in a copolymer of styrene and acrylonitrile, and then dispersed in a hydrocarbon medium.
この方法においては、飽和磁化の高い微粒子を用いてい
るので、マグネタイト磁性流体より高い飽和磁化が期待
されるが、しかし金属微粒子の濃度を高くするとペース
ト状となるため、濃度を増すことができず、３００〜４
００ガウスのものしか得られておらず、結局マグネタイ
ト磁性流体に比較して何等有意な差が認められない。こ
れらを解決するため、特定の界面活性剤を使用すること
により解決を図ったものもあるが、分散安定性について
は十分に満足できるものではなく、特に４０，ＱＯＯＧ
程度の高遠心力下においては沈降を生じる場合もあるの
が現状である。In this method, fine particles with high saturation magnetization are used, so it is expected that the saturation magnetization will be higher than that of magnetite magnetic fluid. However, if the concentration of metal fine particles is increased, it becomes paste-like, so it is not possible to increase the concentration. , 300-4
Only 0.00 Gauss was obtained, and after all, no significant difference was observed compared to magnetite magnetic fluid. Some attempts have been made to solve these problems by using specific surfactants, but the dispersion stability is not fully satisfactory, especially 40, QOOG.
At present, sedimentation may occur under moderately high centrifugal force.
（解決しようとする課題）
したがって、飽和磁化が高く、かつゲル化を起こさず、
約４０，ＯＯＯＧの高遠心力下においても分散性が良好
な磁性流体が開発されれば極めて広い分野においての利
用が可能となる。(Problem to be solved) Therefore, it has high saturation magnetization and does not cause gelation.
If a magnetic fluid with good dispersibility even under high centrifugal force of about 40,000 mm is developed, it will be possible to use it in an extremely wide range of fields.
（課題を解決するための手段）
そこで、本発明者らは、これらの課題を解決すべく鋭意
検討を重ねた結果本発明を完成した。本発明は特定の分
散剤および特定の方法で製造された金属微粒子を使用す
ることにより、従来の磁性流体に比べて格段に優れた分
散安定性および磁化を有する磁性流体組成物を提供する
ものである。(Means for Solving the Problems) Therefore, the present inventors have completed the present invention as a result of intensive studies to solve these problems. The present invention uses a specific dispersant and fine metal particles produced by a specific method to provide a magnetic fluid composition that has significantly superior dispersion stability and magnetization compared to conventional magnetic fluids. be.
すなわち本発明は、コバルトあるいは鉄の金属微粒子と
溶媒と溶媒に可溶の分散剤とを含む磁性流体において、
該金属微粒子がコバルトカルボニルあるいは鉄カルボニ
ルを熱分解して得られたちのであり、かつ前記溶媒に可
溶の分散剤が一般式（１）および（ＩＩ）で表わされる
アルキルまたはアルケニルコハク酸イミド、および一般
式（ＩＩ１）で表わされるベンジルアミンから選ばれる
少なくとも一種から成ることを特徴とする磁性流体組成
物（但し、式中Ｒはアルキル基またはアルケニル基を示
し、 Ｒｌ− は炭素数２〜５の２価の飽和脂肪族炭化
水素基を示し、Ｘはθ〜１０の整数を表わし、そしてｙ
は０−１０の整数を表わす）に存する。That is, the present invention provides a magnetic fluid containing fine metal particles of cobalt or iron, a solvent, and a dispersant soluble in the solvent.
The metal fine particles are obtained by thermally decomposing cobalt carbonyl or iron carbonyl, and the dispersant soluble in the solvent is an alkyl or alkenyl succinimide represented by the general formulas (1) and (II), and A magnetic fluid composition characterized in that it consists of at least one selected from benzylamine represented by the general formula (II1) (wherein R represents an alkyl group or an alkenyl group, and Rl- has 2 to 5 carbon atoms). represents a divalent saturated aliphatic hydrocarbon group, X represents an integer of θ to 10, and y
represents an integer from 0 to 10).
本発明に使用する分散剤のひとつであるアルキルまたは
アルケニルコハク酸イミドは下記一般式ノ
（但し、式中Ｒはアルキル基またはアルケニル基を示し
、 Ｒｌ− は炭素数２〜５の２価の飽和脂肪族炭化水
素基を示し、Ｘは０〜ＩＯの整数を表わす）で表わされ
るものであり、Ｒのアルキル基またはアルケニル基とし
ては通常炭素数５〜２００、好ましくは５０〜１００程
度のものである。The alkyl or alkenyl succinimide, which is one of the dispersants used in the present invention, has the following general formula (wherein R represents an alkyl group or an alkenyl group, and Rl- represents a divalent saturated group having 2 to 5 carbon atoms. represents an aliphatic hydrocarbon group, where X represents an integer from 0 to IO), and the alkyl group or alkenyl group for R usually has about 5 to 200 carbon atoms, preferably about 50 to 100 carbon atoms. be.
Ｒ＋−は、好ましくはエチレン基またはプロピレン基で
あり、さらに好ましくはエチレン基である。R+- is preferably an ethylene group or a propylene group, more preferably an ethylene group.
また上記イミドの望ましい分子量としては８００〜３５
００程度のものである。The desirable molecular weight of the imide is 800 to 35.
It is about 00.
上記イミドは、一般にはボリブテンと無水マレイン酸と
の反応で得られるポリブテニルこはく酸無水物とポリア
ミンとの反応によって合成される。The imide is generally synthesized by reacting polybutenyl succinic anhydride obtained by reacting polybutene with maleic anhydride and a polyamine.
ポリアミンの例としては、単一ノアミン、例えばエチレ
ンジアミン、ブロビレンジアミン、ブチレンノアミンお
よびベンチレンジアミン；ボリアルキレンボリアミン、
例えばジエチレントリアミン、トリエチレンテトラミン
、テトラエヂレンベンタミン、ベンタエチレンへキサミ
ン、ジ（メチルエチレン）トリアミン、ジブチレントリ
アミン、トリブチレンテトラミンおよびペンタベンチレ
ンへキサミン等が挙げられる。Examples of polyamines include single noamines such as ethylene diamine, brobylene diamine, butylene diamine and benchlene diamine; polyalkylene polyamines,
Examples include diethylenetriamine, triethylenetetramine, tetraethylenebentamine, bentaethylenehexamine, di(methylethylene)triamine, dibutylenetriamine, tributylenetetramine, and pentabentylenehexamine.
さらにらうひとつの分散剤であるベンジルアミンはポリ
ブテニルフェノールとホルムアルデヒドとポリアルキレ
ンボリアミンとのマンニッヒ反応によって合成され、次
のような一般式
（但し、式中ＲおよびＲｌは前記に同じ、ｙは０〜１０
の整数である。）で表わされるものである。Furthermore, benzylamine, which is another dispersant, is synthesized by the Mannich reaction of polybutenylphenol, formaldehyde, and polyalkylene polyamine, and has the following general formula (wherein R and Rl are the same as above, y is 0 to 10
is an integer. ).
Ｒのアルキル基またはアルケニル基としては通常炭素数
５〜２００、好ましくは５０〜１００程度の６のである
。好ましいＲ１は、エチレン基またはプロピレン基であ
り、さらに好ましくはエチレン基である。ｙの好ましい
値は２または３である。The alkyl group or alkenyl group for R usually has 6 carbon atoms and has about 5 to 200 carbon atoms, preferably about 50 to 100 carbon atoms. Preferably R1 is an ethylene group or a propylene group, more preferably an ethylene group. A preferred value for y is 2 or 3.
また上記ペンノルアミンの望ましい分子量としては８０
０〜３５００程度のものである。In addition, the desirable molecular weight of the pennolamine is 80.
It is about 0 to 3500.
丑記のペンノルアミンの合成に用いられるポリアミンと
しては、前記したごときポリアミンが同様に用いられる
。As the polyamine used in the synthesis of the pennolamine of Ox, the above-mentioned polyamines are similarly used.
添加するこれらの分散剤は、金属微粒子に対して５〜８
０重ｍ％、好ましくは１３〜６０重Ｍ％である。少ない
と実効かなく、多すぎると反応後沈澱が生じる。These dispersants to be added have a ratio of 5 to 8 to the metal fine particles.
It is 0% by weight, preferably 13 to 60% by weight. If it is too small, it will not be effective, and if it is too large, precipitation will occur after the reaction.
溶媒としては、種々の炭化水素あるいはその混合物が用
いられ、例えばバラフィンお上びオレフィン系炭化水素
の単独あるいは混合物、キンレン、ポリーα−才レフィ
ン、アルキルナフタレン、ケロシン等の鉱油等が挙げら
れる。溶媒は、金属微粒子に対し、５０〜３５０重量％
使用することができる。As the solvent, various hydrocarbons or mixtures thereof can be used, such as paraffin and olefinic hydrocarbons singly or in mixtures, mineral oils such as quince, polyalpha-olefin, alkylnaphthalene, kerosene, and the like. The solvent is 50 to 350% by weight based on the metal fine particles.
can be used.
本発明の磁性流体組成物中のコバルトあるいは鉄の微粒
子径は１０〜！５０Ｘ、好ましくは５０〜１２ｏＸであ
る。コバルトあるいは鉄の濃度は磁性流体組成中、約６
０ｆｆｉ量％以下、好ましくは５５重量％以下である。The particle diameter of cobalt or iron in the magnetic fluid composition of the present invention is 10~! 50X, preferably 50-12oX. The concentration of cobalt or iron is approximately 6
0ffi amount % or less, preferably 55 weight % or less.
多すぎるとゲル化を生じる。金属微粒子は、Ｏ価の金属
であるが、僅かの酸化物を含んでいてもかまわない。Too much amount will cause gelation. The metal fine particles are O-valent metals, but may contain a small amount of oxide.
本発明の磁性流体を作製するには公知の方法で行うこと
ができる。すなわち、分散剤を溶解させた溶媒中に金属
カルボニルを加え、混合溶液を加熱し、金属力ルボニル
の熱分解を行う。金属カルボニルとしては、Ｃｏｗ（Ｃ
ｏ）ａやＦｅ（Ｃｏ）ｓを用いるのが好ましい。また、
熱分解温度は！２０〜１９０℃、熱分解時間は２〜５０
時間であり、温度および時間については、コバルトや鉄
の濃度によって適宜変更すればよい。The magnetic fluid of the present invention can be produced by known methods. That is, a metal carbonyl is added to a solvent in which a dispersant is dissolved, and the mixed solution is heated to thermally decompose the metal carbonyl. As the metal carbonyl, Cow (C
o) It is preferable to use a or Fe(Co)s. Also,
What is the thermal decomposition temperature? 20~190℃, thermal decomposition time is 2~50℃
The temperature and time may be changed as appropriate depending on the concentration of cobalt or iron.
このような磁性流体は、所定の容器に入れ、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
。Preferably, such magnetic fluid is placed in a predetermined container, and the inside of the container is replaced with an inert gas such as argon or nitrogen.
（発明の効果）
本発明の磁性流体は、ＣｏやＦｅという飽和磁化の高い
金属微粒子を用いているため、高い飽和磁化を有すると
ともに、特定の分散剤を用いて、溶媒中に金属微粒子を
分散させているため、約４０．０００Ｇの遠心力下にお
いても沈降せず、極めて高い分散性を有するものである
。また、金属微粒子の濃度を変えることにより、所望の
飽和磁化を有する磁性流体を得ることもできる。(Effects of the Invention) The magnetic fluid of the present invention uses Co and Fe metal fine particles with high saturation magnetization, so it has high saturation magnetization, and the metal fine particles are dispersed in a solvent using a specific dispersant. Because of this, it does not settle even under centrifugal force of about 40,000 G, and has extremely high dispersibility. Further, by changing the concentration of metal fine particles, a magnetic fluid having a desired saturation magnetization can be obtained.
（実施例） 以下に実施例および比較例を示して本発明を説明する。(Example) The present invention will be explained below with reference to Examples and Comparative Examples.
実施例１〜４
分散剤としてアルケニルコハク酸イミド（日本ループリ
ゾール（株）、Ｌｕｂｒｉｚｏｌ ８ ９ ０、窒素ｍ
１．１重量％）５９をケロシン３０９に溶解させた溶液
を冷却器、温度計、ｈガス導入管、撹はん装置をつけた
四ツ目フラスコに入れた。これに、オクタカルボニルコ
バルト［Ｃｏｔ（ＣＯ）ｓ］を５０ｇ加えた。この溶液
を撹拌しながらマントルヒーターで徐々に加熱し、１５
０℃で約２０時間還流を行いながらオクタカルボニルコ
バルトの熱分解を行った。この際、冷却器上部から分解
してできた一酸化炭素が発生する。この一酸化炭素の発
生が終了後、撹拌しながら冷却し、黒色の磁性流体組成
物を得た。Examples 1 to 4 Alkenyl succinimide (Nippon Lubrizol Co., Ltd., Lubrizol 890, nitrogen m
A solution of 1.1% by weight) 59 dissolved in kerosene 309 was placed in a four-eye flask equipped with a condenser, a thermometer, an H gas inlet tube, and a stirrer. To this was added 50 g of octacarbonyl cobalt [Cot(CO)s]. Gradually heat this solution with a mantle heater while stirring.
Octacarbonyl cobalt was thermally decomposed while refluxing at 0° C. for about 20 hours. At this time, decomposed carbon monoxide is generated from the upper part of the cooler. After the generation of carbon monoxide was completed, the mixture was cooled while stirring to obtain a black magnetic fluid composition.
この場合、ケロシン溶媒量を変化させることにより、種
々の磁化を有する磁性Ａ体組成物（実施例１〜４）を得
た。得られた磁性流体組成物の磁化とそこに含まれるコ
バルト濃度の関係を第１表に示す。In this case, magnetic A body compositions (Examples 1 to 4) having various magnetizations were obtained by changing the amount of kerosene solvent. Table 1 shows the relationship between the magnetization of the obtained magnetic fluid composition and the cobalt concentration contained therein.
実施例５〜７
実施例１〜４において、アルケニルコハク酸イミドの替
わりにベンジルアミン（ＡＭＯＣＯ９２５０ （アモコ
社製、窒素量１．１重量％））を用いた以外は同様の方
法にて行った。Examples 5 to 7 Examples 1 to 4 were carried out in the same manner as in Examples 1 to 4, except that benzylamine (AMOCO9250 (manufactured by Amoco, nitrogen content: 1.1% by weight)) was used instead of alkenylsuccinimide.
この場合、ケロシン溶媒量を変化させることにより、３
種の磁化を有する磁性流体組成物（実施例５〜７）を得
た。得られた磁性流体組成物の磁化とそこに含まれるコ
バルト濃度の関係を第２表に示す。In this case, by changing the amount of kerosene solvent, 3
Ferrofluid compositions (Examples 5-7) with seed magnetization were obtained. Table 2 shows the relationship between the magnetization of the obtained magnetic fluid composition and the cobalt concentration contained therein.
実施例８〜１０
実施例１〜４で作製したケロンン溶媒コバルト含有磁性
流体に、実施例８では鉱油（ニュートラル油、１００℃
の粘度３． ４ ０ ｃｓＬ） 、実施例９ではポリ
ーα−オレフィン（ ＩＩＴＥｃ−１６４（日本クーバ
ー社製、１００℃の粘度４ ． Ｏ ｃｓｔ））、そ
して実施例１０ではアルキルナフタレン（炭素数１６と
１８のものの混合物、４０℃の粘度が２９ｃＳｔ）を各
々加え、四ツ目フラスコ中でケロシン溶媒を蒸発させ、
最終的にこの溶液をロータリーエバボレータにかけて、
約１７０〜１８０℃の温度にて軽質溶媒を除去し、各々
磁性流体組成物を得た。Examples 8 to 10 In Example 8, mineral oil (neutral oil, 100°C
Viscosity of 3. 40 csL) in Example 9, a polyα-olefin (IITEc-164 (manufactured by Nippon Cooper Co., Ltd., viscosity at 100°C: 4.0 cst)), and in Example 10 alkylnaphthalene (a mixture of 16 and 18 carbon atoms). , viscosity at 40° C. is 29 cSt), evaporate the kerosene solvent in a four-eye flask,
Finally, apply this solution to a rotary evaporator,
The light solvent was removed at a temperature of about 170-180<0>C to obtain each magnetic fluid composition.
各溶媒での磁化とコバルト濃度の関係の１例を第３表に
示す。Table 3 shows an example of the relationship between magnetization and cobalt concentration in each solvent.
実施例ＩＩおよび１２
実施例１〜４でｃｏｔ（ｃｏ）ｓの替わりに、Ｆｅ（Ｃ
ｏ）ｓを用いた以外は同様の方法によった。この場合、
ケロシン溶媒量を変化させることにより、２種の磁化を
有する磁性流体組成物の磁化とそこに含まれる鉄濃度の
関係を第４表に示す。Examples II and 12 In Examples 1 to 4, instead of cot(co)s, Fe(C
o) The same method was used except that s was used. in this case,
Table 4 shows the relationship between magnetization and iron concentration of magnetic fluid compositions having two types of magnetization by varying the amount of kerosene solvent.
比較例ｌおよび２
実施例ｌ〜４において、分散剤アルケニルコハク酸イミ
ドの替わりに市販の界面活性剤レシチン（リン脂質でホ
スファチジルコリンともいう。）を用いた以外は同様の
方法によった。この場合、ケロシン溶媒量を変化させる
ことにより、２種の磁化を有する磁性流体組成物（比較
例ｌ、２）を得た。得られた磁性流体組成物の磁化とそ
こに含まれるコバルト濃度との関係および分散安定性の
結果を第５表に示す。Comparative Examples 1 and 2 In Examples 1 to 4, the same method was followed except that the commercially available surfactant lecithin (phospholipid, also called phosphatidylcholine) was used instead of the dispersant alkenylsuccinimide. In this case, by varying the amount of kerosene solvent, magnetic fluid compositions with two types of magnetization (Comparative Examples 1 and 2) were obtained. Table 5 shows the relationship between the magnetization of the obtained magnetic fluid composition and the cobalt concentration contained therein, as well as the results of the dispersion stability.
実施例１−１ ２は、２０．０００ ｒｐｉの４４，Ｏ
ＯＯＧ， １時間の遠心分離後においても分離、沈降
等は認められず、極めて優れた分散安定性を示す。Example 1-12 is 44,000 at 20.000 rpi.
OOG, no separation or sedimentation was observed even after centrifugation for 1 hour, indicating extremely excellent dispersion stability.
Claims (1)
可溶の分散剤とを含む磁性流体において、該金属微粒子
がコバルトカルボニルあるいは鉄カルボニルを熱分解し
て得られたものであり、かつ前記溶媒に可溶の分散剤が
一般式（Ｉ）および（II）で表わされるアルキルまたは
アルケニルコハク酸イミド、および一般式（III）で表
わされるベンジルアミンから選ばれる少なくとも一種か
ら成ることを特徴とする磁性流体組成物 ▲数式、化学式、表等があります▼ （ I ） ▲数式、化学式、表等があります▼ （II） ▲数式、化学式、表等があります▼ （III） （但し、式中Ｒはアルキル基またはアルケニル基を示し
、−Ｒ＾１−は炭素数２〜５の２価の飽和脂肪族炭化水
素基を示し、ｘは０〜１０の整数を表わし、そしてｙは
０〜１０の整数を表わす）。(1) A magnetic fluid containing fine metal particles of cobalt or iron, a solvent, and a dispersant soluble in the solvent, in which the metal fine particles are obtained by thermally decomposing cobalt carbonyl or iron carbonyl, and the metal fine particles are obtained by thermally decomposing cobalt carbonyl or iron carbonyl; A magnetic material characterized in that the dispersant soluble in is composed of at least one selected from alkyl or alkenyl succinimides represented by general formulas (I) and (II), and benzylamine represented by general formula (III). Fluid composition ▲ Contains mathematical formulas, chemical formulas, tables, etc. ▼ (I) ▲ Contains mathematical formulas, chemical formulas, tables, etc. ▼ (II) ▲ Contains mathematical formulas, chemical formulas, tables, etc. ▼ (III) (However, R in the formula is alkyl group or alkenyl group, -R^1- represents a divalent saturated aliphatic hydrocarbon group having 2 to 5 carbon atoms, x represents an integer of 0 to 10, and y represents an integer of 0 to 10. ).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP6127489A JPH02239603A (en) | 1989-03-14 | 1989-03-14 | Magnetic fluid composition |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP6127489A JPH02239603A (en) | 1989-03-14 | 1989-03-14 | Magnetic fluid composition |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH02239603A true JPH02239603A (en) | 1990-09-21 |
Family
ID=13166469
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP6127489A Pending JPH02239603A (en) | 1989-03-14 | 1989-03-14 | Magnetic fluid composition |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH02239603A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1996019686A3 (en) * | 1994-12-15 | 1996-10-17 | Ferrotec Corp | Ferrofluid having oxidation resistance |
| EP1329488A1 (en) * | 2000-10-13 | 2003-07-23 | Ulvac, Inc. | Ink-jet ink and process for producing the same |
| EP1349135A4 (en) * | 2000-12-04 | 2005-01-12 | Ulvac Inc | Method of forming electrode for flat panel display |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6211207A (en) * | 1985-07-09 | 1987-01-20 | Natl Res Inst For Metals | Metallic magnetic fluid |
-
1989
- 1989-03-14 JP JP6127489A patent/JPH02239603A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6211207A (en) * | 1985-07-09 | 1987-01-20 | Natl Res Inst For Metals | Metallic magnetic fluid |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1996019686A3 (en) * | 1994-12-15 | 1996-10-17 | Ferrotec Corp | Ferrofluid having oxidation resistance |
| US5656196A (en) * | 1994-12-15 | 1997-08-12 | Ferrotec Corporation | Ferrofluid having improved oxidation resistance |
| US5879580A (en) * | 1994-12-15 | 1999-03-09 | Ferrotec Corporation | Ferrofluid having improved oxidation resistance |
| EP1329488A1 (en) * | 2000-10-13 | 2003-07-23 | Ulvac, Inc. | Ink-jet ink and process for producing the same |
| EP1329488A4 (en) * | 2000-10-13 | 2004-12-01 | Ulvac Inc | Ink-jet ink and process for producing the same |
| EP1349135A4 (en) * | 2000-12-04 | 2005-01-12 | Ulvac Inc | Method of forming electrode for flat panel display |
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