JPH04134353A - Production of spherical magnetic particle - Google Patents
Production of spherical magnetic particleInfo
- Publication number
- JPH04134353A JPH04134353A JP2256279A JP25627990A JPH04134353A JP H04134353 A JPH04134353 A JP H04134353A JP 2256279 A JP2256279 A JP 2256279A JP 25627990 A JP25627990 A JP 25627990A JP H04134353 A JPH04134353 A JP H04134353A
- Authority
- JP
- Japan
- Prior art keywords
- emulsion
- compd
- aqueous solution
- soln
- magnetic 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
- 239000006249 magnetic particle Substances 0.000 title claims abstract description 27
- 238000004519 manufacturing process Methods 0.000 title claims description 13
- 239000000839 emulsion Substances 0.000 claims abstract description 35
- 239000004094 surface-active agent Substances 0.000 claims abstract description 13
- 239000007864 aqueous solution Substances 0.000 claims description 30
- 239000003960 organic solvent Substances 0.000 claims description 13
- 239000000203 mixture Substances 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 150000002484 inorganic compounds Chemical class 0.000 claims description 7
- 229910010272 inorganic material Inorganic materials 0.000 claims description 7
- 239000011790 ferrous sulphate Substances 0.000 claims description 6
- 235000003891 ferrous sulphate Nutrition 0.000 claims description 6
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 6
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 4
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 claims description 4
- 229910000360 iron(III) sulfate Inorganic materials 0.000 claims description 4
- 239000002244 precipitate Substances 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 2
- 239000002904 solvent Substances 0.000 abstract description 6
- 238000004945 emulsification Methods 0.000 abstract description 4
- 238000000034 method Methods 0.000 description 14
- 239000002245 particle Substances 0.000 description 14
- 229940125782 compound 2 Drugs 0.000 description 11
- 238000006243 chemical reaction Methods 0.000 description 9
- 229940125904 compound 1 Drugs 0.000 description 9
- 239000000463 material Substances 0.000 description 7
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- -1 benzene and toluene Chemical class 0.000 description 5
- 239000000969 carrier Substances 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000000889 atomisation Methods 0.000 description 2
- 229940126214 compound 3 Drugs 0.000 description 2
- DIOQZVSQGTUSAI-UHFFFAOYSA-N decane Chemical compound CCCCCCCCCC DIOQZVSQGTUSAI-UHFFFAOYSA-N 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 235000014113 dietary fatty acids Nutrition 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000194 fatty acid Substances 0.000 description 2
- 229930195729 fatty acid Natural products 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 239000002736 nonionic surfactant Substances 0.000 description 2
- 238000010899 nucleation Methods 0.000 description 2
- 230000006911 nucleation Effects 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000010298 pulverizing process Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- XZIIFPSPUDAGJM-UHFFFAOYSA-N 6-chloro-2-n,2-n-diethylpyrimidine-2,4-diamine Chemical compound CCN(CC)C1=NC(N)=CC(Cl)=N1 XZIIFPSPUDAGJM-UHFFFAOYSA-N 0.000 description 1
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 1
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- HVUMOYIDDBPOLL-XWVZOOPGSA-N Sorbitan monostearate Chemical compound CCCCCCCCCCCCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O HVUMOYIDDBPOLL-XWVZOOPGSA-N 0.000 description 1
- ZEEBGORNQSEQBE-UHFFFAOYSA-N [2-(3-phenylphenoxy)-6-(trifluoromethyl)pyridin-4-yl]methanamine Chemical compound C1(=CC(=CC=C1)OC1=NC(=CC(=C1)CN)C(F)(F)F)C1=CC=CC=C1 ZEEBGORNQSEQBE-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000001338 aliphatic hydrocarbons Chemical class 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000001804 emulsifying effect Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 239000002563 ionic surfactant Substances 0.000 description 1
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000244 polyoxyethylene sorbitan monooleate Substances 0.000 description 1
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 description 1
- 229920000053 polysorbate 80 Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 229940035044 sorbitan monolaurate Drugs 0.000 description 1
- 239000001587 sorbitan monostearate Substances 0.000 description 1
- 235000011076 sorbitan monostearate Nutrition 0.000 description 1
- 229940035048 sorbitan monostearate Drugs 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
- H01F1/445—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 compound, e.g. Fe3O4
Abstract
Description
【発明の詳細な説明】
〈産業上の利用分野〉
本発明は、電子写真用トナー、マグネトグラフィー用ト
ナー、各種磁気記録材料、各種キャリアー等、各種工業
に用いられる球状磁性粒子の製造方法に関し、特に、簡
易で粒径制御の容易な球状磁性粒子の製造方法に関する
。[Detailed Description of the Invention] <Industrial Application Field> The present invention relates to a method for producing spherical magnetic particles used in various industries such as electrophotographic toners, magnetography toners, various magnetic recording materials, and various carriers. In particular, the present invention relates to a method for manufacturing spherical magnetic particles that is simple and easy to control particle size.
〈従来技術〉
従来より、磁性粒子は、電子写真用トナー、マグネトグ
ラフィー用トナー、各種磁気記録材料、各種キャリアー
等、各種工業に用いられる。一般に、これらの磁性粒子
は、粒状、針状、板状、薄片状、あるいは棒状等、様々
な形状を有している。<Prior Art> Magnetic particles have conventionally been used in various industries, such as toners for electrophotography, toners for magnetography, various magnetic recording materials, and various carriers. Generally, these magnetic particles have various shapes such as granules, needles, plates, flakes, or rods.
これらを球形化することにより、トナー濃度の上昇、磁
気記録材料の高密度化、担持物質の輸送の効率化等が期
待される。By making these spherical, it is expected that the toner concentration will be increased, the density of the magnetic recording material will be increased, and the transport of the supported substance will be made more efficient.
球状磁性粒子の製造方法として、従来より、水溶液から
の沈殿反応、物理的な粉砕による微粒化等が知られてい
る。（例えば、浜田１ 「表面Ｊ第２５巻第１４７〜１
５７頁（１９８７）） Ｌかし、これらの方法には以下
のような問題点があった。即ち、水溶液からの沈殿反応
による場合は、
■均一水溶液への温度変化や貧溶媒の添加による物理的
状態の変化、あるいは、沈殿剤の添加による化学的変化
によって粒子の構成要素の濃度が過飽和状態となる過程
、
■熱的ゆらぎによって会合した種が安定核として成長す
る過程、
■■で生成した安定核を新たな核生成を起こすことなく
成長させる過程、
■構成、あるいは、再結晶による緩和過程、以上４つの
過程を経て製造されるため、過飽和状態や核生成時間の
制御等極めて厳しい条件設定が必要であり、困難が伴っ
た。また、物理的な粉砕による微粒化の場合は、粒子径
を１μｍ以下にするのは難しく、しかも粒度分布が広い
という問題点があった。As methods for producing spherical magnetic particles, methods such as precipitation reaction from an aqueous solution and atomization by physical pulverization are conventionally known. (For example, Hamada 1 “Surface J Vol. 25 No. 147-1
57 (1987)) However, these methods had the following problems. In other words, in the case of a precipitation reaction from an aqueous solution, the concentration of the constituent elements of the particles reaches a supersaturated state due to a change in the physical state due to a temperature change or the addition of a poor solvent to a homogeneous aqueous solution, or a chemical change due to the addition of a precipitant. ■ A process in which seeds associated by thermal fluctuations grow as stable nuclei; ■ A process in which the stable nuclei generated in ■ grow without new nucleation; ■ A relaxation process due to composition or recrystallization. Since it is manufactured through the above four processes, it is necessary to set extremely strict conditions such as controlling the supersaturation state and nucleation time, which is accompanied by difficulties. Further, in the case of atomization by physical pulverization, it is difficult to reduce the particle size to 1 μm or less, and there is a problem that the particle size distribution is wide.
〈発明が解決しようとする課題〉
本発明は、電子写真用トナー、マグネトグラフィー用ト
ナー、各種磁気記録材料、各種キャリア等、各種工業に
用いられる球状磁性粒子の製造方法に関し、特に、簡易
で粒径制御の容易な球状磁性粒子の製造方法を提供する
ことを目的とする。<Problems to be Solved by the Invention> The present invention relates to a method for producing spherical magnetic particles used in various industries such as toner for electrophotography, toner for magnetography, various magnetic recording materials, and various carriers, and in particular, relates to a method for producing spherical magnetic particles that are simple and granular. The object of the present invention is to provide a method for producing spherical magnetic particles whose diameter can be easily controlled.
〈課題を解決するための手段〉
本発明は、上記目的を達成するためになされたものであ
り、硫酸第一鉄もしくは硫酸第一鉄と硫酸第二鉄の混合
物の水溶液を、有１！ｊ８媒中に油溶性界面活性剤を用
いて乳化分散しＷ／Ｏ型エマルノヨンとし、次いで、該
エマルジョン中の水溶液と反応して磁性粒子を沈殿生成
させる無機化合物の水溶液中に、前記エマルジョンを注
入して、得られた沈澱物を加熱乾燥することを特徴とす
る球状磁性粒子の製造方法である。<Means for Solving the Problems> The present invention has been made in order to achieve the above-mentioned object. The emulsion is emulsified and dispersed in J8 medium using an oil-soluble surfactant to form a W/O emulsion, and then the emulsion is poured into an aqueous solution of an inorganic compound that reacts with the aqueous solution in the emulsion to precipitate magnetic particles. This method of producing spherical magnetic particles is characterized by heating and drying the obtained precipitate.
なお、本発明において、無機化合物の水？８液中にエマ
ルジョンを「注入する」という意味は、エマルジョンの
状態をくずさないように、静かにエマルジョンを無機化
合物の水溶液に注ぎ入れる、ということである。例示的
には、水溶液中に細いガラス管を差し入れ、このガラス
管を通してエマルジョンを少量ずつ水溶液に混入するこ
とが、あげられる。In addition, in the present invention, inorganic compound water? 8. ``Injecting'' an emulsion into a liquid means pouring the emulsion into an aqueous solution of an inorganic compound gently without disturbing the state of the emulsion. An example is to insert a thin glass tube into the aqueous solution and mix the emulsion into the aqueous solution little by little through the glass tube.
本発明の有機溶媒は、それの水に対する溶解度が３重量
％以下であることが好ましい。The organic solvent of the present invention preferably has a solubility in water of 3% by weight or less.
く作用〉
上述の球状磁性粒子の製造方法は、硫酸第一鉄もしくは
硫酸第一鉄と硫酸第二鉄の混合物（以下、化合物１とい
う）の水溶液と有機溶媒からＷ／Ｏ型エマルノヨンを調
製し、次いで、該エマルジョンを該エマルジョン中の水
／８！＆と反応して磁性粒子を沈殿生成させる無機化合
物（以下、化合物２という）の水？８液中に注入する方
法であり、エマルジョン粒子の粒径、形態を保持した球
状磁性粒子（以下、化合物３という）が生成するため、
簡易で粒径制御が容易である。Effect> The method for producing spherical magnetic particles described above involves preparing a W/O type emulsion from an aqueous solution of ferrous sulfate or a mixture of ferrous sulfate and ferric sulfate (hereinafter referred to as compound 1) and an organic solvent. , then the emulsion is mixed with water in the emulsion/8! An inorganic compound (hereinafter referred to as compound 2) that reacts with water to precipitate magnetic particles (hereinafter referred to as compound 2)? 8. This is a method of injecting into a liquid, and spherical magnetic particles (hereinafter referred to as compound 3) that retain the particle size and shape of emulsion particles are generated.
Simple and easy to control particle size.
〈発明の詳細な
説明を図面を用い、以下詳細に説明する。第１図（１）
〜（［［ｌ）は、本発明の製造方法の工程を模式的に表
した説明図である。<Detailed explanation of the invention will be explained in detail below using the drawings. Figure 1 (1)
~([[l] is an explanatory diagram schematically showing the steps of the manufacturing method of the present invention.
工程（Ｉ）：第１図（１）において、化合物ｌの水溶液
と有機溶媒４とを、油溶性界面活性剤５を介して乳化し
、Ｗ／Ｏ型エマルジョンを調製する。Step (I): In FIG. 1 (1), an aqueous solution of compound 1 and an organic solvent 4 are emulsified via an oil-soluble surfactant 5 to prepare a W/O emulsion.
工程（■）：第１図（Ｉｔ）において、工程（Ｉ）で調
製したＷ／Ｏ型エマルジョンを撹拌されている化合物２
の水溶液中に注入し、Ｗ／Ｏ型エマルジョンを分散させ
る。Step (■): In FIG. 1 (It), compound 2 is stirred in the W/O emulsion prepared in step (I).
into an aqueous solution to disperse a W/O emulsion.
工程（■）：第１図（Ｉ［［）において、有機溶媒４が
分離し、油溶性界面活性剤５に包まれた化合物１の水？
８液は、化合物２の水溶液中に放出される。化合物２は
油溶性界面活性剤５相をとおり、液滴表面で化合物１の
水溶液と反応し、球状磁性粒子である化合物３が生成す
る。Step (■): In FIG.
Liquid 8 is released into the aqueous solution of Compound 2. Compound 2 passes through the five oil-soluble surfactant phases and reacts with the aqueous solution of Compound 1 on the surface of the droplet, producing Compound 3 as spherical magnetic particles.
本発明における化合物１は、０．５ｍｏｌ／ｆ以上、飽
和状態以下の濃度であれば使用可能であるが、１ＩＩｌ
ｏＩ／１以上２ｍｏｌ／１以下が好ましい。Compound 1 in the present invention can be used at a concentration of 0.5 mol/f or more and less than the saturation state, but 1IIl
oI/1 or more and 2 mol/1 or less is preferable.
また、本発明で用いられる有Ｉｌ溶媒は、常温で液状で
あり、反応に関与せず水に対する溶解度が３％以下であ
ればよく、ベンゼン、トルエンなどの芳香族炭化水素、
シクロヘキサン等の脂環式炭化水素、ヘキサン、デカン
等の脂肪族炭化水素などが挙げられるがこれらに限定さ
れるものではない、これらの有機溶媒は、単独、あるい
は混合して用いられる。Ｗ／Ｏ型エマルジョンを調製ス
る際の有ｍ熔媒の添加量は、エマルジョンの５０体積％
より多い必要があるが、好ましくは７０体積％〜８０体
積％がよい。乳化方法は、一般の乳化機による方法の他
に、振とう法等を用いることができる。In addition, the Il-containing solvent used in the present invention is liquid at room temperature, does not participate in the reaction, and only needs to have a solubility in water of 3% or less, such as aromatic hydrocarbons such as benzene and toluene,
These organic solvents include, but are not limited to, alicyclic hydrocarbons such as cyclohexane, and aliphatic hydrocarbons such as hexane and decane. These organic solvents may be used alone or in combination. The amount of solvent added when preparing a W/O emulsion is 50% by volume of the emulsion.
Although it needs to be more than 70% by volume to 80% by volume. As the emulsification method, in addition to a method using a general emulsifying machine, a shaking method or the like can be used.
乳化の速度によりエマルジョンの粒径が決定されるため
、種々の速度で行うことができるが、５０００ｒｐ１ｍ
〜／Ｏ０００ｒｐＨ１が好ましい。Since the particle size of the emulsion is determined by the speed of emulsification, it can be carried out at various speeds, but 5000 rpm/m
~/O000rpH1 is preferred.
油溶性界面活性剤としては、ソルビタンモノラウリン酸
エステル等のソルビタン脂肪酸エステルや、ソルビタン
脂肪酸エステルのエチレンオキサイド縮合物等の非イオ
ン性界面活性剤、スルホこはく酸ジー２−エチルへキシ
ルナトリウム等のイオン性界面活性剤が挙げられ、これ
らを単独、あるいは混合して用いられる。界面活性剤の
添加量は、化合物ｌの水溶液の量により適宜決定される
必要があるが、通常は、有機溶媒に対して０．１〜５重
量％が好ましい。Examples of oil-soluble surfactants include sorbitan fatty acid esters such as sorbitan monolaurate, nonionic surfactants such as ethylene oxide condensates of sorbitan fatty acid esters, and ionic surfactants such as di-2-ethylhexyl sodium sulfosuccinate. Examples include surfactants, and these can be used alone or in combination. The amount of surfactant to be added needs to be appropriately determined depending on the amount of the aqueous solution of compound 1, but it is usually preferably 0.1 to 5% by weight based on the organic solvent.
化合物２としては、水溶性であり、化合物１と反応して
沈殿を生成する物質が用いられる。好ましくは、水酸化
ナトリウムがよい。化合物２の添加量は、化合物１の量
によって適宜決定される必要があるが、通常は、０．０
．Ｍｏｌ／ １以上であり、Ｏｌｍｏｌ ／ １〜２ｓ
ｏｌ ／ ｌが好ましい。As Compound 2, a substance that is water-soluble and reacts with Compound 1 to form a precipitate is used. Preferably, sodium hydroxide is used. The amount of compound 2 added needs to be appropriately determined depending on the amount of compound 1, but is usually 0.0
．． Mol/1 or more, Olmol/1~2s
ol/l is preferred.
化合物ｌの水溶液と有機溶媒によるＷ／Ｏ型エマルジョ
ンを化合物２の水溶液に注入する場合は、化合物２の水
溶液は一般の羽根付攪拌機により攪拌されている必要が
あるが、この攪拌速度は、化合物１の水溶液と有ｍ溶媒
を乳化した際の速度より遅くすることが好ましい。When injecting a W/O emulsion consisting of an aqueous solution of Compound 1 and an organic solvent into an aqueous solution of Compound 2, the aqueous solution of Compound 2 must be stirred using a general bladed stirrer; It is preferable to make the emulsification speed slower than the speed at which the aqueous solution of No. 1 and the organic solvent are emulsified.
化合物１の水？８ｅ、と化合物２の水溶液の反応は、通
常常温常圧で進行する。反応は、約１時間で完結する。Compound 1 water? The reaction between 8e and an aqueous solution of compound 2 usually proceeds at room temperature and pressure. The reaction is completed in about 1 hour.
ここで、有ｌ！溶媒４の分離を促し、反応速度を高める
ために加熱するのもよい。加熱温度は、有機溶媒の沸点
以下に設定する必要がある。Here, there is! Heating may also be used to promote separation of the solvent 4 and increase the reaction rate. The heating temperature needs to be set below the boiling point of the organic solvent.
反応終了後、ろ過、あるいは遠心分離により球状磁性粒
子を分離し、水洗、メタノール洗後、加熱乾燥し最終性
成物とする。After the reaction is completed, the spherical magnetic particles are separated by filtration or centrifugation, washed with water and methanol, and then heated and dried to obtain a final product.
以下、本発明を実施例により具体的に説明する。Hereinafter, the present invention will be specifically explained with reference to Examples.
〈実施例〉
１ ｍｏｌ／ １ ｇ酸第−鉄水溶液／Ｏｍ１と１ ｍ
ｏｌ／ １硫酸第二鉄水溶１／Ｏｅｌを混合し、１．５
重量％の非イオン性界面活性剤（ソルビタンモノステア
リン酸エステルとポリオキシエチレンソルビタンモノオ
レイン酸エステルの重量混合比２：１の混合物）ヘンゼ
ン溶液／Ｏ０１に添加し、超高速ホモジナイザー（ポリ
トロン：スイスキネマチイカ社製商品名）を用いて８０
００ｒｐｍで乳化してＷ／○エマルジョンとした。次に
、このＷ／Ｏエマルジョンを３００ｒｐｍで攪拌されて
いる６ ｍｏｌ／ ｊ２の水酸化すＩ・リウム水溶液２
００Ｉ１１中に注入し、１時間撹拌し反応を行った。反
応終了後、生成物を遠心分離機により分離し水洗、メタ
ノール洗した。さらに、９０°Ｃで５時間乾燥し、平均
粒径／Ｏμ−の球状マグネタイトを得た。<Example> 1 mol/1 g ferrous acid aqueous solution/Om1 and 1 m
ol/1 ferric sulfate aqueous solution 1/Oel mixed, 1.5
% by weight of a nonionic surfactant (a mixture of sorbitan monostearate and polyoxyethylene sorbitan monooleate at a weight mixing ratio of 2:1) was added to Hensen's solution/O01, and the mixture was heated using an ultrahigh-speed homogenizer (Polytron: Swiss Cinema). 80 using Chiika product name)
The mixture was emulsified at 00 rpm to form a W/○ emulsion. Next, this W/O emulsion was mixed with a 6 mol/j2 aqueous solution of 2 lithium hydroxide, which was stirred at 300 rpm.
The mixture was poured into 00I11 and stirred for 1 hour to carry out the reaction. After the reaction was completed, the product was separated using a centrifuge and washed with water and methanol. Furthermore, it was dried at 90°C for 5 hours to obtain spherical magnetite with an average particle size of /Oμ.
〈発明の効果〉
本発明は上述のようなものであり、硫酸第一鉄と硫酸第
二鉄の混合物、あるいは、硫酸第一鉄の水溶液を有機溶
媒中に油溶性界面活性剤を介して乳化分散しＷ／Ｏ型エ
マルジョンとし、次に、このエマルジョンをエマルジョ
ン中の水溶液と反応して磁性粒子を沈殿生成させる無機
化合物の水溶液中に注入するという製造方法を用いるこ
とにより、短時間で簡易に球状の磁性粒子を得るこ、と
ができる。また、本発明の製造方法によれば、エマルジ
ョンの粒径に応した粒径の球状磁性粒子が得られるので
あり、エマルジョン作成条件、例えば攪拌の強さ、攪拌
の回転数、界面活性剤の選定等により、粒径の大きさを
制御でき、かつ粒径の揃った球状磁性粒子が得られる。<Effects of the Invention> The present invention is as described above, and emulsifies a mixture of ferrous sulfate and ferric sulfate or an aqueous solution of ferrous sulfate in an organic solvent via an oil-soluble surfactant. By using a production method of dispersing to form a W/O emulsion and then injecting this emulsion into an aqueous solution of an inorganic compound that reacts with the aqueous solution in the emulsion to precipitate magnetic particles, it can be produced easily and in a short time. It is possible to obtain spherical magnetic particles. Furthermore, according to the production method of the present invention, spherical magnetic particles with a particle size corresponding to the particle size of the emulsion can be obtained, and emulsion preparation conditions, such as stirring strength, stirring rotation speed, and selection of surfactant, can be obtained. By such methods, the particle size can be controlled and spherical magnetic particles with uniform particle size can be obtained.
また、粒径の揃った球状磁性粒子は、電子写真用トナー
、マグネトグラフィー用トナー、各種磁気記録材料、各
種キャリアー等、各種工業において、トナー濃度の上昇
、磁気記録材料の高密度化、担持物質の輸送の効率化等
が期待される。In addition, spherical magnetic particles with uniform particle size are used in various industries such as electrophotographic toners, magnetography toners, various magnetic recording materials, and various carriers to increase toner concentration, increase the density of magnetic recording materials, and support materials. This is expected to improve the efficiency of transportation.
第１図（１）〜（Ｉｌｌ）は、本発明の製造方法の各工
程を模式的に示す説明図である。
１・・・化合物１の水溶液
２・・・化合物２の水溶液
３・・・球状磁性粒子
４・・・有機溶媒
５・・・油溶性界面活性剤FIGS. 1(1) to (Ill) are explanatory diagrams schematically showing each step of the manufacturing method of the present invention. 1... Aqueous solution of compound 1 2... Aqueous solution of compound 2 3... Spherical magnetic particles 4... Organic solvent 5... Oil-soluble surfactant
Claims (2)
合物の水溶液を、有機溶媒中に油溶性界面活性剤を用い
て乳化分散しＷ／Ｏ型エマルジョンとし、次いで、該エ
マルジョン中の水溶液と反応して磁性粒子を沈殿生成さ
せる無機化合物の水溶液中に、前記エマルジョンを注入
して、得られた沈澱物を加熱乾燥することを特徴とする
球状磁性粒子の製造方法。(1) An aqueous solution of ferrous sulfate or a mixture of ferrous sulfate and ferric sulfate is emulsified and dispersed in an organic solvent using an oil-soluble surfactant to form a W/O emulsion, and then in the emulsion A method for producing spherical magnetic particles, which comprises injecting the emulsion into an aqueous solution of an inorganic compound that reacts with an aqueous solution of the inorganic compound to precipitate magnetic particles, and heating and drying the obtained precipitate.
あることを特徴とする請求項（１）記載の球状磁性粒子
の製造方法。(2) The method for producing spherical magnetic particles according to claim (1), wherein the organic solvent has a solubility in water of 3% by weight or less.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2256279A JPH04134353A (en) | 1990-09-26 | 1990-09-26 | Production of spherical magnetic particle |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2256279A JPH04134353A (en) | 1990-09-26 | 1990-09-26 | Production of spherical magnetic particle |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH04134353A true JPH04134353A (en) | 1992-05-08 |
Family
ID=17290442
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2256279A Pending JPH04134353A (en) | 1990-09-26 | 1990-09-26 | Production of spherical magnetic particle |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH04134353A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008030975A (en) * | 2006-07-26 | 2008-02-14 | Miyazaki Tlo:Kk | Substance-adsorptive magnetite and its manufacturing method |
| JP2008169110A (en) * | 2001-10-12 | 2008-07-24 | Seoul National Univ Industry Foundation | Method of producing mono-disperse and highly-crystalline nano-particles of metal, alloy, metal oxide, and composite metallic oxide without size-selection process |
| JP2011057473A (en) * | 2009-09-07 | 2011-03-24 | Univ Of Miyazaki | Method for manufacturing magnetite fine particle |
-
1990
- 1990-09-26 JP JP2256279A patent/JPH04134353A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008169110A (en) * | 2001-10-12 | 2008-07-24 | Seoul National Univ Industry Foundation | Method of producing mono-disperse and highly-crystalline nano-particles of metal, alloy, metal oxide, and composite metallic oxide without size-selection process |
| JP2008030975A (en) * | 2006-07-26 | 2008-02-14 | Miyazaki Tlo:Kk | Substance-adsorptive magnetite and its manufacturing method |
| JP2011057473A (en) * | 2009-09-07 | 2011-03-24 | Univ Of Miyazaki | Method for manufacturing magnetite fine particle |
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