JPH01107502A - Manufacture of magnetic fluid - Google Patents

Manufacture of magnetic fluid

Info

Publication number
JPH01107502A
JPH01107502A JP62265049A JP26504987A JPH01107502A JP H01107502 A JPH01107502 A JP H01107502A JP 62265049 A JP62265049 A JP 62265049A JP 26504987 A JP26504987 A JP 26504987A JP H01107502 A JPH01107502 A JP H01107502A
Authority
JP
Japan
Prior art keywords
pulverizing
magnetic fluid
medium
zirconia
diameter
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
JP62265049A
Other languages
Japanese (ja)
Other versions
JP2689251B2 (en
Inventor
Noboru Ichinose
昇 一ノ瀬
Hideaki Honoki
朴木 秀明
Yorio Hirose
広瀬 順夫
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.)
Toshiba Corp
Japan Metals and Chemical Co Ltd
Original Assignee
Toshiba Corp
Japan Metals and Chemical 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 Toshiba Corp, Japan Metals and Chemical Co Ltd filed Critical Toshiba Corp
Priority to JP62265049A priority Critical patent/JP2689251B2/en
Publication of JPH01107502A publication Critical patent/JPH01107502A/en
Application granted granted Critical
Publication of JP2689251B2 publication Critical patent/JP2689251B2/en
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

Links

Classifications

    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/44Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of magnetic liquids, e.g. ferrofluids
    • H01F1/445Magnets 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 compound, e.g. Fe3O4

Landscapes

  • Engineering & Computer Science (AREA)
  • Power Engineering (AREA)
  • Lubricants (AREA)
  • Soft Magnetic Materials (AREA)

Abstract

PURPOSE:To eliminate contamination or the like of magnetic fluid with pulverizing medium, to relatively uniformize ferromagnetic oxide particles, and to obtain the fluid which can be uniformly dispersed in a solvent by pulverizing it with zirconia balls having 0.5-3.0mm of diameter as the pulverizing medium of wet pulverizing. CONSTITUTION:Magnetic fluid in which colloid of ferromagnetic oxide having uniform particles are uniformly dispersed is obtained by pulverizing with zirconia balls having 0.5-3.0mm of diameter as pulverizing medium of wet pulverizing. Used ferromagnetic oxide includes sole or composite ferrite or the like, such as magnetite or Mn, Mn-Zn, Ni-Zn, etc., and the pulverizing medium employs balls having 0.5-3mm of diameter and made of zirconia. Since the zirconia has high hardness and excellent corrosion resistance, contamination due to the wear of the medium does not substantially occur, and since the zirconia itself is of oxide, it does not substantially affect the influence, even if small amount is mixed, to the properties of the magnetic fluid as compared with the medium of metal or alloy. Thus, the fluid which can be employed as various utilities for specific weight sorting, etc., can be simply and inexpensively obtained.

Description

【発明の詳細な説明】 〔産業上の利用分野〕 本発明は磁性流体の製造法であって、湿式粉砕における
粉砕媒体による汚染が少なく、しかも均一、微細な強磁
性体のコロイドからなる磁性流体の製造法に関するもの
である。
[Detailed Description of the Invention] [Field of Industrial Application] The present invention relates to a method for producing a magnetic fluid, which produces a magnetic fluid that is less contaminated by grinding media in wet grinding, and is uniform and made of fine ferromagnetic colloids. This relates to a manufacturing method.

〔従来の技術〕[Conventional technology]

磁性流体は強磁性体微粒子を水又は有機溶媒に懸濁させ
た懸濁液であって、近年医療1表示装置、比重差選別9
回転軸シール等各種用途に利用されている。
A magnetic fluid is a suspension of ferromagnetic fine particles suspended in water or an organic solvent, and in recent years it has been used in medical display devices and specific gravity differential sorting devices.
It is used for various purposes such as rotating shaft seals.

従来、磁性流体は、マグネタイト(Fe304)コロイ
ドが主として用いられている。
Conventionally, magnetite (Fe304) colloids have been mainly used as magnetic fluids.

その製造方法は、(l)マグネタイトをオレイン酸を含
む有機層中でボールミル粉砕した後大きな粒子を分離す
る湿式粉砕法、(2)湿式マグネタイトに水溶液中でオ
レイン酸イオンを吸着させ、水洗脱水後分散処理する水
溶液中吸着−有機層分散法、(3)第1鉄塩と第2鉄塩
の混合水溶液にアルカリ添加後オレイン酸を含む加゛熱
ケロシン中に添加する解膠法などが提案されて゛いるO また、磁性流体としては、マグネタイトのような強磁性
酸化物のコロイドの他に、強磁性金属、合金又は化合物
のコロイド等も提案されている(特公昭61−3936
9号公報)。
The manufacturing method is (l) a wet pulverization method in which magnetite is ball milled in an organic layer containing oleic acid and then large particles are separated; (2) oleate ions are adsorbed on wet magnetite in an aqueous solution, and after washing and dehydration. The adsorption-organic layer dispersion method in an aqueous solution for dispersion treatment, and (3) peptization method in which alkali is added to a mixed aqueous solution of ferrous and ferric salts and then added to heated kerosene containing oleic acid have been proposed. In addition to colloids of ferromagnetic oxides such as magnetite, colloids of ferromagnetic metals, alloys, or compounds have also been proposed as magnetic fluids (Japanese Patent Publication No. 61-3936
Publication No. 9).

蕊に、磁性流体においては、溶媒に懸濁さ九ている強磁
性粉末は、懸濁液を安定せしめるため、100〜200
Aの微粒子であること及び粒径が可及的に均一であるこ
とを必要としている。
In magnetic fluids, the ferromagnetic powder suspended in the solvent has a concentration of 100 to 200 to stabilize the suspension.
It is necessary that the particles be A fine particles and that the particle size be as uniform as possible.

本発明は、強磁性粉末として金属酸化物強磁性体(フェ
ライト)を用い、湿式粉砕による方法に関するものであ
るが、一般Vこ強磁性酸化物等の粉砕はボールミル等を
用いた湿式粉砕法が採用されており、例えば特開昭58
−110431号の方法はフェライトな超硬合金からな
るボールミルで粉砕するものである。
The present invention relates to a wet pulverization method using a metal oxide ferromagnetic material (ferrite) as a ferromagnetic powder, but a wet pulverization method using a ball mill or the like is generally used for pulverizing ferromagnetic oxides. For example, JP-A-58
The method of No. 110431 involves grinding with a ball mill made of ferritic cemented carbide.

〔本発明が解決しようとする問題点〕[Problems to be solved by the present invention]

前述、従来の方法において、ポールミルヲ用いて湿式粉
砕する方法は粉砕処理が簡単であるが、粗大粒径のもの
を含むため、磁性流体に使用するためにはこれを濾過酸
るいは遠心分離などによってそれを除く必要がある。
As mentioned above, in the conventional method of wet pulverization using a pole mill, the pulverization process is simple, but since it contains coarse particles, in order to use it for magnetic fluids, it is necessary to process it by filtration, pickling, centrifugation, etc. It is necessary to remove it.

また、比較的長時間の粉砕となるため、粉砕媒体の摩耗
によって生ずる不純物の混入が避けられないという欠点
がある。
Furthermore, since the grinding takes a relatively long time, there is a drawback that contamination with impurities caused by wear of the grinding media is unavoidable.

本発明は前述従来法の欠点を改善するため研究の結果強
磁性酸化物を湿式粉砕によって粉砕することによって粉
砕媒体による汚染等がなく、しかも強磁性酸化物粒子が
比較的均一にでき、それによって溶媒中に均一に分散で
きる磁性流体の製造法を提供することにある。
In order to improve the drawbacks of the conventional method mentioned above, the present invention has been made as a result of research and has resulted in pulverizing ferromagnetic oxide by wet pulverization, thereby eliminating contamination by the pulverizing media and making the ferromagnetic oxide particles relatively uniform. An object of the present invention is to provide a method for producing a magnetic fluid that can be uniformly dispersed in a solvent.

〔問題点を解決するための手段〕[Means for solving problems]

本発明は強磁性酸化物を界面活性剤を溶解した溶媒中で
湿式粉砕して磁性流体を製造する方法において、前記湿
式粉砕の粉砕媒体として直径0.5〜3.0mmのジル
コニアボールを用いて粉砕することによって、均一粒子
の強磁性酸化物のコロイドを均一に分散させた磁性流体
の製造法である。
The present invention provides a method for manufacturing a magnetic fluid by wet-pulverizing a ferromagnetic oxide in a solvent in which a surfactant is dissolved, using zirconia balls having a diameter of 0.5 to 3.0 mm as a grinding medium for the wet grinding. This is a method for producing a magnetic fluid in which colloidal ferromagnetic oxide particles are uniformly dispersed by pulverization.

〔作  用〕[For production]

本発明は以上の如き構成のものからなり、芸で使用する
強磁性酸化物は、マグネタイト又はMn、 Mn−Zn
、 Ni−Zn等の単元又は複合フェライト等であり、
粉砕媒体はジルコニア製の直径0.5〜3朋のボールを
使用する。ジルコニアは非常に硬く、耐触性に優れてい
るため、粉砕媒体の摩耗による汚染は殆んどなく、また
ジルコニア自体が酸化物であることにより、金属又は合
金製の粉砕媒体と比較して、多少混入しても磁性流体の
性質に殆んど影響しない。
The present invention has the above structure, and the ferromagnetic oxide used in the art is magnetite, Mn, Mn-Zn.
, unitary or composite ferrite such as Ni-Zn,
As the grinding medium, zirconia balls with a diameter of 0.5 to 3 mm are used. Zirconia is very hard and has excellent corrosion resistance, so there is almost no contamination due to abrasion of the grinding media, and since zirconia itself is an oxide, compared to grinding media made of metals or alloys, Even if some amount of it is mixed in, it will hardly affect the properties of the magnetic fluid.

ジルコニアボールの粒径な0.5〜3.0mmとするの
は湿式粉砕時に被粉砕物の粒径の分布を適正範囲内で均
一なものとすることができるからである。
The reason why the particle size of the zirconia balls is set to 0.5 to 3.0 mm is that the particle size distribution of the material to be ground can be made uniform within an appropriate range during wet grinding.

さらに、本発明における湿式粉砕において使用する装置
は、公知の各種装置が使用でき、また溶媒は磁性流体と
して一般に用いられている水又はケロシン、ヘプタン、
ヘキサン、エステル類、フルオロカーボン類等の各種有
機溶媒が使用できる。
Furthermore, various known devices can be used for the wet grinding of the present invention, and the solvent can be water, kerosene, heptane, etc., which are commonly used as magnetic fluids.
Various organic solvents such as hexane, esters, and fluorocarbons can be used.

また、前記磁性酸化物粒子を溶媒中に懸濁させるために
各種の界面活性剤を使用する。その界面活性剤は該強磁
性酸化物に対し吸着性を有するものであって、例えばオ
レイン酸、リノール酸若しくはコハク酸等の各種脂肪酸
のほかアニオン界面活性剤、カチオン界面活性剤、非イ
オン界面活性剤等が使用できる。尚、この場合界面活性
剤はその溶媒に応じて各種の界面活性剤を適宜採択すれ
ばよい。
Additionally, various surfactants are used to suspend the magnetic oxide particles in the solvent. The surfactant has adsorption properties to the ferromagnetic oxide, and includes various fatty acids such as oleic acid, linoleic acid, and succinic acid, as well as anionic surfactants, cationic surfactants, and nonionic surfactants. Agents etc. can be used. In this case, various surfactants may be appropriately selected depending on the solvent.

本発明は以上のように従来のボールミルによる湿式粉砕
法と同様に簡単に磁性流体を得ることができると共に、
従来の湿式粉砕法にも簡単に適用できる。
As described above, the present invention allows magnetic fluid to be easily obtained in the same way as the conventional wet grinding method using a ball mill, and
It can also be easily applied to conventional wet grinding methods.

また、本発明によって得られる強磁性酸化物は粒径も微
細で、かつ均一なものであるから、従来の如き粗大粒子
の分離除去処理の必要は全くない。
Furthermore, since the ferromagnetic oxide obtained by the present invention has fine and uniform particle sizes, there is no need for the conventional separation and removal treatment of coarse particles.

さらに、本発明によって得られる磁性流体は100〜1
50人の範囲の均一なコロイドが均一に分散されたもの
として得られるため、比重差選別9回転軸シールその他
各種の用途に広く適用することができる。
Furthermore, the magnetic fluid obtained by the present invention has a 100 to 1
Since a uniform colloid with a range of 50 particles is obtained as a uniformly dispersed product, it can be widely applied to various applications such as specific gravity selection, 9 rotary shaft seals, and others.

〔実 施 例〕〔Example〕

以下、実施例をもって本発明を具体的に説明する。 The present invention will be specifically explained below with reference to Examples.

実施例1 マグネタイト粉末100grを、20grのリノール酸
を含有したケロシン200m/中で、直径1龍のジルコ
ニアボールを媒体としたボールミルを用いて12週間粉
砕したところ8kOeの磁場中で約150ガウスの磁化
を持つ磁性流体が得られた。
Example 1 100g of magnetite powder was pulverized for 12 weeks in 200ml of kerosene containing 20g of linoleic acid using a ball mill using zirconia balls with a diameter of 1 dragon as a medium, resulting in a magnetization of about 150 Gauss in a magnetic field of 8kOe. A magnetic fluid with .

実施例2 マグネタイト粉末300grを、90grのオレイン酸
を含有したケロシン600m/中で、直径2朋のジルコ
ニアボールを媒体としたボールミルを用いて10週間粉
砕した。次にこの液体を直径0.5朋のジルコニアボー
ルを用いたアトリッションミルにより8日間粉砕したと
ころ、約180ガウスの磁化を持つ磁性流体が得られた
Example 2 300g of magnetite powder was ground for 10 weeks in 600ml of kerosene containing 90g of oleic acid using a ball mill using zirconia balls with a diameter of 2mm as a medium. Next, when this liquid was pulverized for 8 days using an attrition mill using zirconia balls with a diameter of 0.5 mm, a magnetic fluid with a magnetization of about 180 Gauss was obtained.

実施例3 炭酸マンガン粉末、亜鉛華、酸化鉄粉末を組成比がMn
o、54Zno、4sFezoaとなるように混合した
ものを、大気中1300℃で3時間焼成した後、窒素雰
囲気下で冷却し、振動ミルで粉砕してMn−Znフェラ
イト粉末を調製した。この試料をオレイン酸及びケロシ
ンを用いて、実施例2のマグネタイトと全く同様の処理
を施したところ、約160ガウスの磁化を持つ磁性流体
が得られた。
Example 3 Manganese carbonate powder, zinc white powder, and iron oxide powder with a composition ratio of Mn
A mixture of ZnO, 54Zno, and 4sFezoa was fired in the air at 1300°C for 3 hours, cooled in a nitrogen atmosphere, and ground in a vibration mill to prepare Mn-Zn ferrite powder. When this sample was treated in exactly the same manner as the magnetite of Example 2 using oleic acid and kerosene, a magnetic fluid having a magnetization of about 160 Gauss was obtained.

〔発明の効果〕〔Effect of the invention〕

以上の如く本発明は強磁性酸化物を用いた磁性流体の製
造に当り、特定粒径のジルコニアボールを用いて湿式粉
砕することによって、強磁性酸化物を適正範囲内に均一
に分散することができ、回転軸シール、比重差選別等各
種用途に二側用できる磁性流体を簡単に、かつ低廉に提
供することができる。
As described above, in producing a magnetic fluid using a ferromagnetic oxide, the present invention makes it possible to uniformly disperse the ferromagnetic oxide within an appropriate range by wet grinding using zirconia balls of a specific particle size. This makes it possible to easily and inexpensively provide a magnetic fluid that can be used on two sides for various purposes such as rotary shaft sealing and specific gravity separation.

特許出願人 −ノ  瀬    昇 同   日本重化学工業株式会社 同 株式会社東芝Patent applicant Noboru Sase Same as Japan Heavy Chemical Industry Co., Ltd. Same as Toshiba Corporation

Claims (1)

【特許請求の範囲】[Claims]  強磁性酸化物を、界面活性剤を溶解した溶媒中で湿式
粉砕して磁性流体を製造する方法において、前記湿式粉
砕の粉砕媒体として直径0.5〜3.0mmのジルコニ
アボールを用いて粉砕することを特徴とする磁性流体の
製造法。
In a method for manufacturing a magnetic fluid by wet-pulverizing a ferromagnetic oxide in a solvent in which a surfactant is dissolved, zirconia balls having a diameter of 0.5 to 3.0 mm are used as the grinding medium for the wet-pulverization. A method for producing a magnetic fluid characterized by:
JP62265049A 1987-10-20 1987-10-20 Magnetic fluid manufacturing method Expired - Fee Related JP2689251B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP62265049A JP2689251B2 (en) 1987-10-20 1987-10-20 Magnetic fluid manufacturing method

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP62265049A JP2689251B2 (en) 1987-10-20 1987-10-20 Magnetic fluid manufacturing method

Publications (2)

Publication Number Publication Date
JPH01107502A true JPH01107502A (en) 1989-04-25
JP2689251B2 JP2689251B2 (en) 1997-12-10

Family

ID=17411872

Family Applications (1)

Application Number Title Priority Date Filing Date
JP62265049A Expired - Fee Related JP2689251B2 (en) 1987-10-20 1987-10-20 Magnetic fluid manufacturing method

Country Status (1)

Country Link
JP (1) JP2689251B2 (en)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2000023192A1 (en) * 1998-10-22 2000-04-27 Ferrofluidics Corporation Method and apparatus for recycling ferrofluid constituents used in a materials separation process
CN103310939A (en) * 2013-05-17 2013-09-18 大连大学 Magnetic liquid using plasma for strengthening magnetism and preparation method thereof
CN108831663A (en) * 2018-06-06 2018-11-16 冀中能源集团有限责任公司 A kind of preparation method and its device of ore dressing magnetic fluid

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5685801A (en) * 1979-12-14 1981-07-13 Matsushita Electric Ind Co Ltd Method of manufacturing oxide semiconductor material for thermistor
JPS59105093A (en) * 1982-12-08 1984-06-18 Nippon Seiko Kk Magnetic fluid composition and its preparation

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5685801A (en) * 1979-12-14 1981-07-13 Matsushita Electric Ind Co Ltd Method of manufacturing oxide semiconductor material for thermistor
JPS59105093A (en) * 1982-12-08 1984-06-18 Nippon Seiko Kk Magnetic fluid composition and its preparation

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2000023192A1 (en) * 1998-10-22 2000-04-27 Ferrofluidics Corporation Method and apparatus for recycling ferrofluid constituents used in a materials separation process
US6103107A (en) * 1998-10-22 2000-08-15 Ferrofluidics Corporation System for recycling ferrofluid constituents used in a materials separation process
US6254781B1 (en) 1998-10-22 2001-07-03 Ferrofluidics Corporation Method for recycling ferrofluid constituents used in a materials separation process
CN103310939A (en) * 2013-05-17 2013-09-18 大连大学 Magnetic liquid using plasma for strengthening magnetism and preparation method thereof
CN103310939B (en) * 2013-05-17 2016-04-06 大连大学 A kind of plasma helps magnetic liquid and preparation method thereof
CN108831663A (en) * 2018-06-06 2018-11-16 冀中能源集团有限责任公司 A kind of preparation method and its device of ore dressing magnetic fluid

Also Published As

Publication number Publication date
JP2689251B2 (en) 1997-12-10

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