JPS60229306A - Surface treatment of magnetic powder and manufacture thereof - Google Patents
Surface treatment of magnetic powder and manufacture thereofInfo
- Publication number
- JPS60229306A JPS60229306A JP59085545A JP8554584A JPS60229306A JP S60229306 A JPS60229306 A JP S60229306A JP 59085545 A JP59085545 A JP 59085545A JP 8554584 A JP8554584 A JP 8554584A JP S60229306 A JPS60229306 A JP S60229306A
- Authority
- JP
- Japan
- Prior art keywords
- group
- magnetic
- magnetic powder
- compound
- molecule
- 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
Links
- 239000006247 magnetic powder Substances 0.000 title claims abstract description 55
- 238000004519 manufacturing process Methods 0.000 title claims description 7
- 238000004381 surface treatment Methods 0.000 title claims description 4
- -1 silane compound Chemical class 0.000 claims abstract description 33
- 239000007822 coupling agent Substances 0.000 claims abstract description 17
- 150000002148 esters Chemical class 0.000 claims abstract description 11
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical group [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000003960 organic solvent Substances 0.000 claims abstract description 7
- 150000003609 titanium compounds Chemical class 0.000 claims abstract description 4
- 229910019142 PO4 Inorganic materials 0.000 claims description 22
- 239000010452 phosphate Substances 0.000 claims description 22
- 150000001875 compounds Chemical class 0.000 claims description 13
- 125000004432 carbon atom Chemical group C* 0.000 claims description 6
- 125000002947 alkylene group Chemical group 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 150000002430 hydrocarbons Chemical group 0.000 claims description 4
- 125000002252 acyl group Chemical group 0.000 claims description 3
- 125000002467 phosphate group Chemical group [H]OP(=O)(O[H])O[*] 0.000 claims description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical group OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 abstract description 17
- 238000000034 method Methods 0.000 abstract description 14
- 239000000843 powder Substances 0.000 abstract description 13
- 229910000077 silane Inorganic materials 0.000 abstract description 8
- 229910052782 aluminium Inorganic materials 0.000 abstract description 6
- 230000003301 hydrolyzing effect Effects 0.000 abstract 3
- 125000003545 alkoxy group Chemical group 0.000 abstract 1
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical group [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 abstract 1
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 36
- 239000011230 binding agent Substances 0.000 description 23
- 239000003973 paint Substances 0.000 description 20
- 235000021317 phosphate Nutrition 0.000 description 20
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 17
- 150000003014 phosphoric acid esters Chemical class 0.000 description 17
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 12
- 238000000576 coating method Methods 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 12
- 239000011248 coating agent Substances 0.000 description 10
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 9
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 description 8
- 239000000203 mixture Substances 0.000 description 8
- 239000010936 titanium Substances 0.000 description 7
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 6
- 239000003795 chemical substances by application Substances 0.000 description 6
- 229920002635 polyurethane Polymers 0.000 description 6
- 239000004814 polyurethane Substances 0.000 description 6
- 229910052719 titanium Inorganic materials 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 239000002904 solvent Substances 0.000 description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 239000000956 alloy Substances 0.000 description 4
- 229910045601 alloy Inorganic materials 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- WRKCIHRWQZQBOL-UHFFFAOYSA-N octyl dihydrogen phosphate Chemical compound CCCCCCCCOP(O)(O)=O WRKCIHRWQZQBOL-UHFFFAOYSA-N 0.000 description 4
- 235000012424 soybean oil Nutrition 0.000 description 4
- 239000003549 soybean oil Substances 0.000 description 4
- 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 3
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 229910001030 Iron–nickel alloy Inorganic materials 0.000 description 3
- 239000006087 Silane Coupling Agent Substances 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 229920001577 copolymer Polymers 0.000 description 3
- 239000002270 dispersing agent Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000004907 flux Effects 0.000 description 3
- 235000010445 lecithin Nutrition 0.000 description 3
- 239000000787 lecithin Substances 0.000 description 3
- 229940067606 lecithin Drugs 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 229920005749 polyurethane resin Polymers 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- 239000004094 surface-active agent Substances 0.000 description 3
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 2
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 2
- 229920002433 Vinyl chloride-vinyl acetate copolymer Polymers 0.000 description 2
- 238000005299 abrasion Methods 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 125000000217 alkyl group Chemical group 0.000 description 2
- 150000001412 amines Chemical class 0.000 description 2
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 238000003490 calendering Methods 0.000 description 2
- 239000007795 chemical reaction product Substances 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- JTXUVYOABGUBMX-UHFFFAOYSA-N didodecyl hydrogen phosphate Chemical compound CCCCCCCCCCCCOP(O)(=O)OCCCCCCCCCCCC JTXUVYOABGUBMX-UHFFFAOYSA-N 0.000 description 2
- 125000000524 functional group Chemical group 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 238000004898 kneading Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000000178 monomer Substances 0.000 description 2
- FDPIMTJIUBPUKL-UHFFFAOYSA-N pentan-3-one Chemical compound CCC(=O)CC FDPIMTJIUBPUKL-UHFFFAOYSA-N 0.000 description 2
- 239000002985 plastic film Substances 0.000 description 2
- 229920000139 polyethylene terephthalate Polymers 0.000 description 2
- 239000005020 polyethylene terephthalate Substances 0.000 description 2
- 229920002689 polyvinyl acetate Polymers 0.000 description 2
- 239000011118 polyvinyl acetate Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000004576 sand Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- DLYUQMMRRRQYAE-UHFFFAOYSA-N tetraphosphorus decaoxide Chemical compound O1P(O2)(=O)OP3(=O)OP1(=O)OP2(=O)O3 DLYUQMMRRRQYAE-UHFFFAOYSA-N 0.000 description 2
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 2
- 229920002554 vinyl polymer Polymers 0.000 description 2
- OEPOKWHJYJXUGD-UHFFFAOYSA-N 2-(3-phenylmethoxyphenyl)-1,3-thiazole-4-carbaldehyde Chemical compound O=CC1=CSC(C=2C=C(OCC=3C=CC=CC=3)C=CC=2)=N1 OEPOKWHJYJXUGD-UHFFFAOYSA-N 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- 239000004593 Epoxy Substances 0.000 description 1
- 239000001856 Ethyl cellulose Substances 0.000 description 1
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 description 1
- NTIZESTWPVYFNL-UHFFFAOYSA-N Methyl isobutyl ketone Chemical compound CC(C)CC(C)=O NTIZESTWPVYFNL-UHFFFAOYSA-N 0.000 description 1
- UIHCLUNTQKBZGK-UHFFFAOYSA-N Methyl isobutyl ketone Natural products CCC(C)C(C)=O UIHCLUNTQKBZGK-UHFFFAOYSA-N 0.000 description 1
- 229920000459 Nitrile rubber Polymers 0.000 description 1
- 239000000020 Nitrocellulose Substances 0.000 description 1
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 1
- 239000004952 Polyamide Substances 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- BZHJMEDXRYGGRV-UHFFFAOYSA-N Vinyl chloride Chemical class ClC=C BZHJMEDXRYGGRV-UHFFFAOYSA-N 0.000 description 1
- MEESPVWIOBCLJW-KTKRTIGZSA-N [(z)-octadec-9-enyl] dihydrogen phosphate Chemical compound CCCCCCCC\C=C/CCCCCCCCOP(O)(O)=O MEESPVWIOBCLJW-KTKRTIGZSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 229920000180 alkyd Polymers 0.000 description 1
- 150000003973 alkyl amines Chemical class 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- YTFJQDNGSQJFNA-UHFFFAOYSA-N benzyl dihydrogen phosphate Chemical compound OP(O)(=O)OCC1=CC=CC=C1 YTFJQDNGSQJFNA-UHFFFAOYSA-N 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000003869 coulometry Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 239000001177 diphosphate Substances 0.000 description 1
- XPPKVPWEQAFLFU-UHFFFAOYSA-J diphosphate(4-) Chemical compound [O-]P([O-])(=O)OP([O-])([O-])=O XPPKVPWEQAFLFU-UHFFFAOYSA-J 0.000 description 1
- 235000011180 diphosphates Nutrition 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- LNTZHXQMPUKVNX-UHFFFAOYSA-N docosyl dihydrogen phosphate Chemical compound CCCCCCCCCCCCCCCCCCCCCCOP(O)(O)=O LNTZHXQMPUKVNX-UHFFFAOYSA-N 0.000 description 1
- TVACALAUIQMRDF-UHFFFAOYSA-N dodecyl dihydrogen phosphate Chemical compound CCCCCCCCCCCCOP(O)(O)=O TVACALAUIQMRDF-UHFFFAOYSA-N 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 235000019325 ethyl cellulose Nutrition 0.000 description 1
- 229920001249 ethyl cellulose Polymers 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- PHNWGDTYCJFUGZ-UHFFFAOYSA-N hexyl dihydrogen phosphate Chemical compound CCCCCCOP(O)(O)=O PHNWGDTYCJFUGZ-UHFFFAOYSA-N 0.000 description 1
- 229920001519 homopolymer Polymers 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 230000033444 hydroxylation Effects 0.000 description 1
- 238000005805 hydroxylation reaction Methods 0.000 description 1
- 239000012442 inert solvent Substances 0.000 description 1
- 239000012948 isocyanate Substances 0.000 description 1
- 210000003127 knee Anatomy 0.000 description 1
- 210000002414 leg Anatomy 0.000 description 1
- 150000004668 long chain fatty acids Chemical class 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229920001220 nitrocellulos Polymers 0.000 description 1
- 239000005486 organic electrolyte Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- AJCDFVKYMIUXCR-UHFFFAOYSA-N oxobarium;oxo(oxoferriooxy)iron Chemical compound [Ba]=O.O=[Fe]O[Fe]=O.O=[Fe]O[Fe]=O.O=[Fe]O[Fe]=O.O=[Fe]O[Fe]=O.O=[Fe]O[Fe]=O.O=[Fe]O[Fe]=O AJCDFVKYMIUXCR-UHFFFAOYSA-N 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 229920006255 plastic film Polymers 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 description 1
- 229920002239 polyacrylonitrile Polymers 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229920006267 polyester film Polymers 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 239000004848 polyfunctional curative Substances 0.000 description 1
- 229920005862 polyol Polymers 0.000 description 1
- 150000003077 polyols Chemical class 0.000 description 1
- 229920000915 polyvinyl chloride Polymers 0.000 description 1
- 239000004800 polyvinyl chloride Substances 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000010526 radical polymerization reaction Methods 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 238000010079 rubber tapping Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229910000702 sendust Inorganic materials 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 125000004079 stearyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
- 229910000859 α-Fe Inorganic materials 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
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
- H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
- H01F1/06—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys in the form of particles, e.g. powder
- H01F1/061—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys in the form of particles, e.g. powder with a protective layer
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は１表面被覆された磁性粉およびその製造方法に
関する。更に詳しくは、ある特定の化合物で表面処理さ
れて、分散性とバインダーとの接着性が改善された磁性
粉およびその製造方法に関する。DETAILED DESCRIPTION OF THE INVENTION [Industrial Field of Application] The present invention relates to a one-surface coated magnetic powder and a method for producing the same. More specifically, the present invention relates to a magnetic powder whose surface is treated with a specific compound to improve dispersibility and adhesion to a binder, and a method for producing the same.
磁気テープ、磁気ディスクなどの磁気記録媒体中の磁性
粉は高度の分散性が要求される。Magnetic powder in magnetic recording media such as magnetic tapes and magnetic disks is required to have a high degree of dispersibility.
磁気記録媒体は一般に、磁性粉末、バインダー、各種添
加剤及び溶剤を混練することによシ鯛造される磁性塗料
をプラスチックのフィルムやシートの基板上に均一に塗
布して乾燥し、その後磁性層を鏡面仕上げして形成され
るが、ｉｎ性塗料中の磁性粉を十分に分散解膠して凝集
粒子を除いておかないと充填密度の大きな均一で平滑な
磁性層を作ることはできない。Generally, magnetic recording media are produced by kneading magnetic powder, a binder, various additives, and solvents, then applying a magnetic paint uniformly onto a plastic film or sheet substrate and drying it. However, unless the magnetic powder in the ink coating is sufficiently dispersed and peptized to remove aggregated particles, it is not possible to create a uniform and smooth magnetic layer with a high packing density.
磁性粉の凝集粒子による磁性層の不拘−Ｆｉ磁気テープ
の！磁変換特性及び磁気特性ＫＭ大な悪影響を及ばず。Unrestricted magnetic layer due to agglomerated particles of magnetic powder - Fi magnetic tape! No major adverse effects on magnetic conversion characteristics and magnetic characteristics KM.
即ち出力の低下、ノイズの増大、ドロップアウトなどの
原因となる。又、磁性粉末とバインダーとの接着力が弱
い場合は。That is, it causes a decrease in output, an increase in noise, dropouts, etc. Also, if the adhesive force between the magnetic powder and the binder is weak.
磁気記録媒体と記録ヘッド又は再生ヘッドとの摺動の際
に、磁性ｊ＆農層からの磁性粉の剥離（いわゆる”粉落
ち”）が起こり易く、塗膜表面が荒れて５ｇｉ気記録媒
体の耐久性が損われる。When a magnetic recording medium and a recording head or a reproducing head slide, magnetic powder tends to peel off from the magnetic layer (so-called "powder falling off"), and the surface of the coating becomes rough, reducing the durability of the recording medium. Sexuality is damaged.
従来の磁気記録媒体においては、かかる耐久性が不十分
のまま火剤化されているのが実状であった。In reality, conventional magnetic recording media have been made into explosives without sufficient durability.
このようＫｔＢ性塗料中の磁性粉の分散性及びバインダ
ーとの接着性は磁気記録媒体の性能を向上させる土で非
常に１！要である。As described above, the dispersibility of the magnetic powder in the KtB paint and the adhesion with the binder are extremely good for improving the performance of magnetic recording media! It is essential.
磁性粉の分散性の向上に関しては種々の観点から研究さ
れておシ、磁性塗料配合に適当な界面活性剤を加えて分
散性を改良することが提案されている。このような界面
活性剤としてはアルキルイミダシリン化合物を用いるも
の（特開昭５４−５２ｓｏ４）、アルキルポリオキシエ
チレンリン酸エステルをアルキルアミンで中和して用い
るもの（特開昭５５−７８８１０）、長鎖アルキルリン
酸エステルを用いるもの（％開開５４−１４７５０７
、 ％ｉｉ昭５５−４９６２９）などのようにアミンと
その誘導体、リン酸エステル、ポリオキシエチレンリン
酸エステル類などを利用することが多い。ｄｌた、磁性
粉を表面処理してから塗料化すると分散性が改良される
とする提案があり、アルキルポリオキシエチレンリン酸
エステルを用いるもの（特開昭５４−９４５０８、同５
６−４９７６９）、メタル粉をチタンカップリング剤で
処理して分散安定性を計ると同時に磁性塗膜の経時劣化
を防ぐもの（％開開５６−８８４７１）などがある。又
、磁性粉とバインダーとの接着性を向上させて磁性塗膜
の耐久性向上を計る方法としては、バインダーと反応性
の官能基をもつシランカップリング剤を用いるもの（特
開昭５４−７５１０）、アミンファンクショナルシラン
カップリング剤とイソシアネート系化合物、エポキシ系
化合物との反応生成物によって被覆するもの（特開昭５
６−１４５５５５）、バインダー中の二重結合とラジカ
ル重合が可能な不飽和結合を南するチタンカップリング
剤で磁性粉を処理するもの（特開昭５６−１１１１２９
）、分子中に少なくとも４個の放射線感応性アクリル系
二重結合を有する化合物をバインダーとして用いるもの
（％開開５７−４０７４４）などがある。このように、
磁性塗料中の磁性粉末の分散性及び磁性塗膜の耐久性の
向上に関して、多くの研究がなされて′ｆＡたにもかか
わらず、朱だに満足すべき改良の段階には到達していな
い。Improvements in the dispersibility of magnetic powder have been studied from various viewpoints, and it has been proposed to improve the dispersibility by adding a suitable surfactant to the magnetic paint formulation. Such surfactants include those using alkylimidacillin compounds (Japanese Patent Laid-Open No. 54-52so4), and those using alkyl polyoxyethylene phosphates neutralized with alkyl amines (Japanese Patent Laid-Open No. 55-78810). , those using long-chain alkyl phosphate esters (% opening 54-147507
In many cases, amines and their derivatives, phosphoric acid esters, polyoxyethylene phosphoric esters, etc. are used. There is also a proposal that the dispersibility is improved by surface-treating magnetic powder and then turning it into a paint, and there is a proposal that uses alkyl polyoxyethylene phosphate ester (JP-A-54-94508, JP-A-54-94508, JP-A-54-94508;
6-49769), and one that treats metal powder with a titanium coupling agent to measure dispersion stability and at the same time prevent the deterioration of the magnetic coating film over time (% opening 56-88471). In addition, as a method for improving the durability of the magnetic coating film by improving the adhesiveness between the magnetic powder and the binder, a method using a silane coupling agent having a functional group reactive with the binder (Japanese Patent Laid-Open No. 54-7510 ), one coated with a reaction product of an amine functional silane coupling agent, an isocyanate compound, and an epoxy compound (JP-A-5
6-145555), a method in which magnetic powder is treated with a titanium coupling agent that binds double bonds in the binder and unsaturated bonds capable of radical polymerization (JP-A-56-111129).
), and those using a compound having at least four radiation-sensitive acrylic double bonds in the molecule as a binder (% open area 57-40744). in this way,
Although much research has been carried out on improving the dispersibility of magnetic powder in magnetic coatings and the durability of magnetic coatings, no satisfactory improvements have been reached yet.
ｃ問題点を解決するための手段〕
本発明者らは、上記の磁気記録媒体の問題点Ｉｃ鑑み、
磁性粉末の分散性とバインダーとの接着性に関して鋭意
研究の結果、特定のリン酸エステルと、特定のカンプリ
ング剤で表面処理された磁性粉が１分散性とパインター
との接着性が著しく向上することを見い出し本発明を完
成したものである。Means for Solving Problem c] In view of the problem Ic of the above magnetic recording medium, the present inventors have
As a result of extensive research into the dispersibility of magnetic powder and its adhesion with binders, we found that magnetic powder surface-treated with a specific phosphoric acid ester and a specific compulsing agent has significantly improved dispersibility and adhesion with pinters. This discovery has led to the completion of the present invention.
即ち１本発明は （１） 次の一般式。That is, the present invention is (1) The following general formula.
［ＲＯ（人０） ］ ＰＯ（ＯＨ）３−。[RO (person 0)] PO (OH) 3-.
ｌ
（式中、ＲＦｉ炭素数２〜２８の炭化水素基又はアシル
基を表わし、Ａ蝶炭素数２〜４のアルキレン基を表わし
、ｎは０又Ｖｉ１〜５０の整数を表し、／ｌ′１１．１
，５又は２ｆｔ表わす）で表わされるリン酸エステル、
および。l (wherein, RFi represents a hydrocarbon group or acyl group having 2 to 28 carbon atoms, A represents an alkylene group having 2 to 4 carbon atoms, n represents 0 or an integer from 1 to 50, /l'11 .1
, 5 or 2 ft);
and.
（ｍｌ −分子中に二個以上のリン酸基金１する分子Ｊ
ｉ；１００００以下のリン酸エステル。(ml - molecule J with two or more phosphate groups in the molecule
i; Phosphoric acid ester of 10,000 or less.
かちなる群よシ選ばれる１８１又は２釉以上のリン酸エ
ステルと。With 181 or 2 or more phosphoric acid esters selected from the Kachinaru group.
（匍 −分子中に加水分解性アルコキシシラン基を有す
る有機シラン化合物。(Sou - An organic silane compound having a hydrolyzable alkoxysilane group in the molecule.
（５）−分子中に加水分解性チタン＆を有する有機チタ
ン化合物、および、
（ｖ）−分子中に加水分解性アルコキシアルミニウム基
を有する有機アルミニウム化合物。(5) - An organotitanium compound having a hydrolyzable titanium & in the molecule, and (v) - An organoaluminum compound having a hydrolyzable alkoxyaluminum group in the molecule.
からなる群よシ選ばれる１種又は２ｓ１以上のカップリ
ング剤、
とによって表面処理された磁性粉を提供するものである
。The present invention provides magnetic powder surface-treated with one or more coupling agents selected from the group consisting of:
本発明の表面処理磁性粉は、前記（１）および（Ｈ）か
らなる群よシ遺ばれる１種又は２種以上のリン酸エステ
ルと、前記（Ｉｔ、吹］およびｆｆＪ ２＞”−らなる
群よｐ選ばれる１種又は２８以上のカップリング剤の両
方を用いて磁性粉を不活性有機電媒中で加熱処理するこ
とにょＩ）得ることができる。The surface-treated magnetic powder of the present invention consists of one or more phosphoric acid esters from the group consisting of the above (1) and (H), and the above (It, blow) and ffJ 2>"- I) can be obtained by heating magnetic powder in an inert organic electrolyte using one or both of 28 or more coupling agents selected from the group.
本発ＢＡｔｔｃ係わる前記（１）のリン酸エステルは、
リン酸とＲ素数２〜２８の炭化水素基をもするヒドロキ
シ化１１あるいはその低級アルキレンオキサイド付加峻
から１１８尋されるリン酸モノエステル、リン酸ジエス
テル又はリン酸セスキエステル、或いはリン酸とＲ素数
２〜２８の脂肪酸又はその低級アルキレンオキサイド付
加物から誘導されるリン酸モノエステル、リン酸ジエス
テル又はリン酸セスキエステルが例示される。The above (1) phosphoric acid ester related to the present BAttc is:
Phosphoric acid monoester, phosphoric acid diester or phosphoric acid sesquiester formed by hydroxylation 11 or its lower alkylene oxide addition steeply comprising phosphoric acid and a hydrocarbon group having an R prime number of 2 to 28, or phosphoric acid and an R prime number Examples include phosphoric acid monoesters, phosphoric acid diesters, and phosphoric acid sesquiesters derived from 2 to 28 fatty acids or their lower alkylene oxide adducts.
具体的な化合物としては、モノドデシルポスフェート、
モノベンジルホスフェート、ジドデシルホスフェート、
セスキドデシルホスフェート。Specific compounds include monododecyl phosphate,
Monobenzyl phosphate, didodecyl phosphate,
Sesquidodecyl phosphate.
セスキベンジルホスフェート、セスキプロピルホスフェ
ート、セスキオクチルホスフェート、セスキオレイルホ
スフェート、モノベヘニルホスフェート、モノへキシル
ホスフェート、ジドデシルホスフェート、モノオレイル
ホスフェート、セスキドデシルポリオキシエチレン（３
）ホスフェート、セスキドデシルポリオキシエチレン（
９）ホスフェート、セスキノニルフェニルポリオキシエ
チレンα１ホスフエート、モノドデシルポリオキシエチ
レン（５）ホスフェート、モノオクタデシルポリオキシ
エチレン（５）ホスフェート、セスキオクタデシルポリ
オキシエチレン峙ホスフェート、セスキオクチルフェニ
ルポリオキシエチレンａａホスフェート、ジオクチルポ
リオキシエチレン（６１ホスフエート、セスキドデシル
ポリオキシプロピレン（９）ホスフェート、モノオクチ
ルポリオキシエチレンαａホスフェート、モノオクタデ
セニルポリオキシプロピレン（８）ホスフェｃ、 、Ｈ
，５ＣＯＯ（ＯＨ２０Ｈ２ｏ）、 ５ＰＯ（ＯＨ）２、
（０５Ｈ，、Ｃ００（ＯＨ２ＣＨ２０）２〕２ＰＯ（Ｏ
Ｈ）等を例示することができる。Sesquibenzyl phosphate, sesquipropyl phosphate, sesquioctyl phosphate, sesquioleyl phosphate, monobehenyl phosphate, monohexyl phosphate, didodecyl phosphate, monooleyl phosphate, sesquidodecyl polyoxyethylene (3
) phosphate, sesquidodecyl polyoxyethylene (
9) phosphate, sesquinonylphenylpolyoxyethylene α1 phosphate, monododecylpolyoxyethylene (5) phosphate, monooctadecylpolyoxyethylene (5) phosphate, sesquioctadecylpolyoxyethylene diphosphate, sesquioctylphenylpolyoxyethylene aa phosphate, Dioctylpolyoxyethylene (61 phosphate, sesquidodecylpolyoxypropylene (9) phosphate, monooctylpolyoxyethylene αa phosphate, monooctadecenylpolyoxypropylene (8) phosphate c, , H
,5COO(OH20H2o), 5PO(OH)2,
(05H,,C00(OH2CH20)2]2PO(O
H) etc. can be exemplified.
本発明に係わる前記（幻のリン酸エステルは。The above (phantom phosphoric acid ester) according to the present invention is.
−分子中にリン酸基（ここでリン酸基とは。-Phosphate group in the molecule (what is a phosphate group here?
１ −ｐｏ （ＯＨ）２又は−ｐｏ（ＯＨ） を意味する。1 -po (OH)2 or -po(OH).
）を２個以上有する分子量１００００以下の化合物であ
シ、その例としては。) with a molecular weight of 10,000 or less, examples thereof include:
（１） ポリエチレングリコール、ポリグロピレングリ
コール、ビスフェノールＡのようなポリオール類あるい
はそれらの低級アルキレンオキサイド付加物とリン酸か
ら誘導されるリン酸エステル、
（２１ヒドロキシ（メタ）アクリレート、ポリオキシエ
チレン（メタ）アクリＬ／−）、Ｎ−ヒドロキシエチル
（メタ）アクリレート、ポリ酢酸ビニルの部分鹸化物な
どの水酸基含有ビニルモノマー成分を含むホモ重合体又
は共重合体と無水リン酸から誘導されるリン酸エステル
。(1) Phosphate esters derived from polyols such as polyethylene glycol, polyglopylene glycol, bisphenol A or their lower alkylene oxide adducts and phosphoric acid, (21 hydroxy (meth)acrylate, polyoxyethylene (meth) ) Acrylic L/-), N-hydroxyethyl (meth)acrylate, partially saponified polyvinyl acetate, and other homopolymers or copolymers containing hydroxyl group-containing vinyl monomer components, and phosphoric acid esters derived from phosphoric anhydride. .
等をあげることができる。etc. can be given.
本発明に係わる前記（匍の有機シラン化合物は分子中に
加水分解性アルコキシン２ン基を有するものであれば特
に限定されず、反応性官能基を有するもの、有しないも
のいずれでもよい。The above-mentioned organic silane compound according to the present invention is not particularly limited as long as it has a hydrolyzable alkoxine group in its molecule, and it may be one with or without a reactive functional group.
これらの化合物を例示すると、（ｃＨ，）２ｓｉ（ｏｃ
Ｈ，）、。Examples of these compounds include (cH,)2si(oc
H, ),.
０Ｈ２＝ＯＨ８ｉ（Ｏｃｉ２Ｈ５）、、 ０Ｈ２＝Ｃ（
ＯＨ，）−Ｃ０００，Ｈ６５１（ＯＯＨ５＞５゜Ｈ２Ｎ
Ｃ２Ｈ４ＮＨＯ３Ｈ６Ｓｉ （ＯＣｒ（３） ３． Ｈ
２ＮＣ２Ｈ４ＮＨＣ；、Ｈ６ＢＩＣＣＨ，）（ＣｉＯＨ
，）２゜Ｈ２Ｎｏ、Ｈ６５ｉ（ＱＣ２Ｈ５）３，８２Ｎ
０ＯＮＨＣ，）Ｉ６Ｓｉ（ＱＣ２Ｈ５）５゜（ＯＨＯ）
ＳｉＣＨＮＨＣＯＮＨＯ６Ｈ，２ＮＣ０。0H2=OH8i(Oci2H5),, 0H2=C(
OH,)-C000,H651(OOH5>5゜H2N
C2H4NHO3H6Si (OCr(3) 3.H
2NC2H4NHC;, H6BICCH,) (CiOH
,)2゜H2No, H65i (QC2H5) 3,82N
0ONHC,)I6Si(QC2H5)5゜(OHO)
SiCHNHCONHO6H,2NC0.
５５５６
（ＯＨ３０）３ＳｉＯ，Ｈ６ＮＨＯ２Ｈ４ＮＨＣＯＮＨ
Ｏ６Ｈ１２Ｎｅｏ 。5556 (OH30)3SiO,H6NHO2H4NHCONH
O6H12Neo.
ＯＨ３
ＣＯ
フェニル又ハアルキルトリアルコキシシラン１モルと長
鎖脂肪酸１〜２モルとの反応生成物、等をあげることが
できる。OH3 CO A reaction product of 1 mole of phenyl or haalkyltrialkoxysilane and 1 to 2 moles of long chain fatty acid, etc. can be mentioned.
本発明に係わる前記−の有機チタン化合物としては、
ａＨ（ｏＨ，）２−ｏ−Ｔｉ（ｏｏｏ−ｃ、Ｈ，５）２
゜ＯＨ３
ＯＨ３
０Ｈ（ＯＨ，）２−ＯＴｉ＋００２Ｈ４ＮＨＯ２Ｈ４Ｎ
Ｈ２）５゜等をあげることができる。The organic titanium compound of - according to the present invention is aH(oH,)2-o-Ti(ooo-c, H,5)2
゜OH3 OH3 0H(OH,)2-OTi+002H4NHO2H4N
H2) 5° etc. can be raised.
また１本発明に係わる前記（Ｖ）の有機アルミニウム化
合物としては
等の化合物を例示することができる。Further, examples of the organic aluminum compound (V) according to the present invention include the following compounds.
本発明に係わる磁性粉末としては針状形の微細なｒ−Ｆ
ｅ２０． 、 Ｆｅ３Ｏ４，０ｒｂ２ のような金属酸
化物、また００被着ｒ−Ｆａ２０３１０ｏドープｒ−Ｆ
ｅ２０゜のよ５な加工処理を施したγ−Ｆｅ２０．、鉄
メタル粉、微小板状のバリウムフェライトおよびそのＦ
ｅ原子の一部がＴｉ１００ｃＺｎ、Ｖ、Ｎｌ）等の１種
または２種以上で置換された磁性粉、００．Ｆｅ−００
，Ｆｅ−Ｎｉ等の金属または合金の超微粉などが挙げら
れる。これらのうち鉄メタル粉は特に化学的安定性が悪
いからこの改良のためニッケル、コノ（ルト、チタン、
ケイ素、アルミニウムなどを金ｊｉｉＩｊＡ子、塩およ
び酸化物の形で少蓋加えた夛表面処理されることがある
がこれらを用いることもできる。鉄メタル粉は寸たその
安定化のため弱い酸化性雰囲気の中で表面に薄い酸化被
膜を作らせることがあるが、このように処理されたメタ
ル粉を用いることもできる。The magnetic powder according to the present invention includes needle-shaped fine r-F.
e20. , Fe3O4,0rb2, and also 00 deposited r-Fa20310o doped r-F
γ-Fe20. , iron metal powder, platelet barium ferrite and its F
Magnetic powder in which a part of e atoms are substituted with one or more of Ti100cZn, V, Nl), etc., 00. Fe-00
, ultrafine powder of metal or alloy such as Fe-Ni. Among these, iron metal powder has particularly poor chemical stability, so in order to improve this, nickel, metal powder, titanium,
The surface may be treated with a small amount of silicon, aluminum, or the like in the form of gold, salt, or oxide, but these may also be used. In order to stabilize the size of iron metal powder, a thin oxide film is sometimes formed on the surface in a weakly oxidizing atmosphere, but metal powder treated in this way can also be used.
特忙、本発明の処理方法によれば、従来高度の分散性を
達成さすことが困難とされていた粒子径１００Ａ〜７０
０Ｘの球状メタル粉や球状合金粉（超微粉）を用いても
高度の分散性を達成させることが可能となる。According to the processing method of the present invention, particle sizes of 100A to 70A, which were conventionally considered difficult to achieve, have a high degree of dispersibility.
Even if 0X spherical metal powder or spherical alloy powder (ultrafine powder) is used, it is possible to achieve a high degree of dispersibility.
本発明の表面処理磁性粉の製造においては、不活性有機
溶媒中で磁性粉を前記リン酸エステルと前記シラン又は
チタン又はアルミニウムカップリング剤を用いて加熱処
理を行う。また必要に応じてさらに加圧してもよい。こ
の場合、リン酸エステルとシラン又はチタン又はアルミ
ニウムカップリング剤の使用ｔは共に磁性粉１００重量
部に対して０．５重量部以上とすることが好ましい。使
用量が０．５重量部未満では、処理磁性粉の性能がやや
不十分となる。また、これら両化合物の使用量比（重量
比）も、リン酸エステル二カップリング剤＝１：５〜５
：１の範囲が好ましい。本発明の製造方法において使用
される不活性有機溶媒は、磁性粉、前記リン酸エステル
およびカップリング剤のいずれとも反応しないものであ
れば使用することが可能であシ、たとえば、メチルエチ
ルケトン、メチルイソブチルケトン、ジエチルケトン、
シクロヘキサノン、ベンゼン、キシレン、トルエン等を
あげることができる。In producing the surface-treated magnetic powder of the present invention, the magnetic powder is heat-treated in an inert organic solvent using the phosphoric acid ester and the silane, titanium, or aluminum coupling agent. Moreover, further pressure may be applied if necessary. In this case, it is preferable that both the phosphoric acid ester and the silane or titanium or aluminum coupling agent be used in an amount of 0.5 parts by weight or more based on 100 parts by weight of the magnetic powder. If the amount used is less than 0.5 part by weight, the performance of the treated magnetic powder will be somewhat insufficient. In addition, the usage ratio (weight ratio) of both these compounds is also phosphoric acid ester di-coupling agent = 1:5 to 5.
: The range of 1 is preferable. The inert organic solvent used in the production method of the present invention can be any solvent as long as it does not react with any of the magnetic powder, the phosphoric acid ester, and the coupling agent, such as methyl ethyl ketone, methyl isobutyl ketone, diethyl ketone,
Examples include cyclohexanone, benzene, xylene, and toluene.
加熱処理温度は６ＤＣ以上とすることが好ましい。処理
温度の上限は特に限定しないが、結局、使用する有機不
活性溶媒の還流温度となるであろう。また、特にＣｏ被
被着−Ｆｅ２Ｏ２は高温で表面が変質することがらるの
で注意を要する。The heat treatment temperature is preferably 6 DC or higher. The upper limit of the treatment temperature is not particularly limited, but will ultimately be the reflux temperature of the organic inert solvent used. In addition, care must be taken especially when Co-coated Fe2O2 is used, as its surface may deteriorate at high temperatures.
また、加熱処理を行う場合の磁性粉、リン酸エステルお
よびカップリング剤の混合順序については特に限定され
ず、たとえば
イ）不活性有機溶媒中に磁性粉（１）、リン酸エステル
（１）およびカップリング剤（１１υを一括混合し加熱
処理を行う方法、
口）不活性有機溶媒中に先ず（１）と（ＩＪを入れて加
熱処理し、その後（１）を追加してさらに加熱処理をす
る方法、あるいは。In addition, the order of mixing the magnetic powder, phosphate ester, and coupling agent when performing heat treatment is not particularly limited. For example, a) magnetic powder (1), phosphate ester (1), and Coupling agent (method of mixing 11υ all at once and heat-treating) First, put (1) and (IJ) in an inert organic solvent and heat-treat, then add (1) and heat-treat. method or.
ハ）不活性有機溶媒中に先ず（１）と（１）を入れて加
熱処理し、その後（Ｉｆ）を追加してさらに加熱処理を
する方法、
のいずれでもよい。(c) First, (1) and (1) are placed in an inert organic solvent and heat-treated, and then (If) is added and further heat-treated.
本発明の磁性粉にバインダーおよび溶剤を加えて塗料化
し、これをポリエステル等のフィルムに塗布することＫ
よりａ気記録媒体とすることができる。K
It is possible to make the recording medium more airy.
処理磁性粉を塗料化する際に用いられるバインダーは有
機溶剤に可溶な樹脂バインダーであシ、上記の磁性粉を
基板上におよび磁性粉同志を必要な強さで固着して磁性
層とするためにできるだけ少量でその役割をはたすもの
であればよく、従来塗料中の磁性粉の分散性を悪化する
懸念のあるものも通常の塗料化方法で用いることができ
る。これらの樹脂バインダーの例としてはポリウレタン
、ポリエステル、ポリ塩化ビニル、塩化ビニル酢酸ビニ
ル共重合体、ポリアクリルニトリル、ニトリルゴム、エ
ポキシ樹脂。The binder used when turning the treated magnetic powder into a paint is a resin binder that is soluble in organic solvents, and the above magnetic powder is fixed onto a substrate and the magnetic powders together with the necessary strength to form a magnetic layer. For this reason, it is sufficient to use a material that can fulfill its role in as small a quantity as possible, and even materials that are concerned about worsening the dispersibility of magnetic powder in conventional paints can be used in normal paint-forming methods. Examples of these resin binders are polyurethane, polyester, polyvinyl chloride, vinyl chloride vinyl acetate copolymer, polyacrylonitrile, nitrile rubber, and epoxy resin.
アルキッド樹脂、ポリアミド、ポリアクリル酸エステル
、ポリメタクリル酸エステル、ポリ酢酸ビニル、ポリビ
ニルブチラール、塩化ビニリデン、塩化ビニリデン共重
合体、硝化綿、マレイン酸変性塩化ビニル／酢酸ビニル
共重合体、エチルセルロースなどが挙げられる。これら
は単独で用いてもよいが、通常２種類以上混合して用い
られる。また樹脂の硬さを調節するため可塑剤や硬化剤
を加えて使用することもできる。Examples include alkyd resin, polyamide, polyacrylic ester, polymethacrylic ester, polyvinyl acetate, polyvinyl butyral, vinylidene chloride, vinylidene chloride copolymer, nitrified cotton, maleic acid-modified vinyl chloride/vinyl acetate copolymer, and ethyl cellulose. It will be done. Although these may be used alone, two or more types are usually used in combination. Further, in order to adjust the hardness of the resin, a plasticizer or a hardening agent may be added.
またバインダーの配合量は一般に磁性粉１００重量部に
対して１５〜６０重量部である。最も大きな結合力を有
するバインダーであっても１５重量部よ多少ないときは
磁性塗膜の強度が弱くまた基板と磁性塗膜の接着力が不
足となる。Further, the amount of the binder blended is generally 15 to 60 parts by weight per 100 parts by weight of the magnetic powder. Even if the binder has the highest binding strength, if it is less than 15 parts by weight, the strength of the magnetic coating will be weak and the adhesive strength between the substrate and the magnetic coating will be insufficient.
また６０重量部よル多いときは磁性ｍｓ中の磁性粉濃度
が／Ｊ％きくなって再生出力が低下して不利であるし、
また塗膜特性が低下することもある。Also, if the amount is more than 60 parts by weight, the concentration of magnetic powder in the magnetic ms becomes /J%, which is disadvantageous because the reproduction output decreases.
Furthermore, the properties of the coating film may deteriorate.
塗料化に用いられる溶剤は使用するバインダーに対して
溶解力を有しかつ沸点が５０Ｃから１５０Ｃの間にある
ものが望ましい。沸点が低すぎると塗布後磁性粉の磁場
配向する前に乾燥してしまいこの処理をすることができ
ない。バインダーの種類に対応して上記の観点から選択
されるが毒性や環境の問題を考慮して選ぶべきことはい
うまでもない。It is desirable that the solvent used for forming the paint has a dissolving power for the binder used and a boiling point between 50C and 150C. If the boiling point is too low, the coating will dry before the magnetic powder is oriented in the magnetic field after coating, making this treatment impossible. The binder is selected from the above viewpoints depending on the type of binder, but it goes without saying that it should be selected in consideration of toxicity and environmental issues.
Ｃ実施例及び効果〕
以下実施例をもって本発明を更に詳しく説明するが本発
明はこれらの実施例に限定されるものではない。C Examples and Effects] The present invention will be explained in more detail with reference to Examples below, but the present invention is not limited to these Examples.
実施例１ 冷却管付５００１セパラブルフラスコＩｃ、Ｃ。Example 1 5001 separable flask with cooling tube Ic, C.
被着ｒ−Ｆｅ２０． （長軸径０．５５μｍ、軸比１／
１０）１５０Ｆ、トルエン５００／、有機シラン化合お
よびセスキドデシルポリオキシエチレン（９モルＭｈｏ
）ホスフェ−）６ＦＬｌ’Ｌ、７５Ｃ〜ａＳＣで２時間
攪拌した。次いで、過剰のトルエンで磁性物を洗浄し、
減圧下６０Ｃに保ちトルエンを除去し、表面処理磁性粉
末を得た。該処理磁性粉末と、バインダーとして塩化ビ
ニル−酢酸ビニルコポリマー（米国のユニオンカーバイ
ド社製のＶＡＧＨ）とホリウレタン樹脂（日本ポリウレ
タン工業株式会社製のニラポラン２５０４）との１：１
（ｉ！ｊｔ比）の混合物を磁性粉末九対して２５ｍ！量
チ及び？Ｖ剤としてメチルエチルケトンとシクロヘキサ
ノンの１＝１（重量比）の混合物１５０Ｉを混合してボ
ールミルで４８時間混練した後、硬化剤（日本ポリウレ
タン工業（株）のコロネートＬ）１０ｊｌを添加して系
か均一になるまで攪拌することにより磁性塗料を得た。Deposited r-Fe20. (long axis diameter 0.55 μm, axial ratio 1/
10) 150F, toluene 500/, organosilane compound and sesquidodecyl polyoxyethylene (9 mol Mho
) Phosphe-)6FLl'L, stirred at 75C to aSC for 2 hours. Then, wash the magnetic material with excess toluene,
The toluene was removed under reduced pressure at 60C to obtain surface-treated magnetic powder. A 1:1 mixture of the treated magnetic powder and a vinyl chloride-vinyl acetate copolymer (VAGH manufactured by Union Carbide, USA) and a polyurethane resin (Niraporan 2504 manufactured by Nippon Polyurethane Industries, Ltd.) as a binder was used.
(i!jt ratio) mixture of 9 magnetic powders and 25m! Quantity and? As a V agent, 150 I of a mixture of methyl ethyl ketone and cyclohexanone in a 1=1 (weight ratio) was mixed and kneaded in a ball mill for 48 hours, and then 10 jl of a curing agent (Coronate L from Nippon Polyurethane Industries Co., Ltd.) was added to make the system homogeneous. A magnetic paint was obtained by stirring the mixture until it became .
この磁性塗料を厚さ１２μｍの強化ポリエチレンテレフ
タレートフィルム上に乾燥膜厚７μａ ＶＣなるように
塗布し、出湯配向してから乾旅し、次いでカレンダー処
理にょシ鏡面加工を施した後、所定の幅に裁断して磁気
テープを得た。該磁気テープにつき、角型比、残留磁束
密度を測定した。また耐摩耗性を、模擬ヘッドを用いて
９０分間０．８ｍ／Ｓｅｃの速さで摺動させてテープ表
面の摩耗度を目測と顕微鏡観察によって判定した。それ
らの結果は表−１に示す。This magnetic paint is applied onto a reinforced polyethylene terephthalate film with a thickness of 12 μm to a dry film thickness of 7 μa VC, oriented after tapping, dried, and then calendered to give it a mirror finish. It was cut to obtain magnetic tape. The squareness ratio and residual magnetic flux density of the magnetic tape were measured. Abrasion resistance was determined by sliding the tape at a speed of 0.8 m/Sec for 90 minutes using a simulated head, and by visual measurement and microscopic observation of the degree of wear on the tape surface. The results are shown in Table-1.
実施例２〜６
表−２に示すリン酸エステルとカンプリング剤を用いて
、実施例１で使用したＣＯ被着ｒ−Ｆθ２０３１５０
、Ｐの表面を実施例１の方法に準じて処理し、処理磁性
粉末、磁性塗料および磁気テープを得た。該磁気テープ
につき実施例１に準じて角型比、残留磁束密度の測定、
耐摩耗性の評価を行った。それらの結果は表−１に示す
。Examples 2 to 6 Using the phosphoric acid ester and camping agent shown in Table 2, the CO deposited r-Fθ203150 used in Example 1 was prepared.
, P was treated according to the method of Example 1 to obtain treated magnetic powder, magnetic paint, and magnetic tape. Measurement of the squareness ratio and residual magnetic flux density of the magnetic tape according to Example 1;
Abrasion resistance was evaluated. The results are shown in Table-1.
実施例７
実施例１で用いた表面処理磁性粉１００重量部、ニトロ
セルロース系バインダー（タイセル化学工業（株）のＦ
Ｍ−２００）１０重量部、ポリウレタン樹脂（日本ポリ
ウレタン工業（株）のニラポラン２３０４）１０重量部
、溶媒としてメチルエチルケトン１ｂＯＭ葉部、シクロ
ヘキサノン８０重量部およびトルエン８０重量部からな
る混合物をボールミルで７２時間混練した後、硬化剤（
日本ポリウレタン工業（株）のコロネートＬ）１０Ｆを
添加して系が均一になるまて攪拌することによシ磁性塗
料を得た。Example 7 100 parts by weight of the surface-treated magnetic powder used in Example 1, nitrocellulose binder (F from Taicel Chemical Industry Co., Ltd.)
M-200), 10 parts by weight of polyurethane resin (Nilaporan 2304 from Nippon Polyurethane Industries Co., Ltd.), methyl ethyl ketone 1bOM leaf as a solvent, 80 parts by weight of cyclohexanone, and 80 parts by weight of toluene were kneaded in a ball mill for 72 hours. After that, add a hardener (
A magnetic paint was obtained by adding Coronate L) 10F (Nippon Polyurethane Industry Co., Ltd.) and stirring until the system became homogeneous.
この磁性塗料を厚さ１２７ＪＩＢ の強化ポリエチレン
テレフタレートフィルム上に乾燥膜厚４μｍになるよう
に塗布し、磁場配向してから乾燥し、次いでカレンダー
処理によシ鏡面加工を施した後、所定の幅に裁断して磁
気テープを得た。該磁気テープにつき実施例１に示した
５項目の測定、評価を行った。それらの結果Ｆｉ表−１
に示す。This magnetic paint was applied to a reinforced polyethylene terephthalate film with a thickness of 127 JIB to a dry film thickness of 4 μm, oriented in a magnetic field, dried, and then calendered to give it a mirror finish. It was cut to obtain magnetic tape. The five items shown in Example 1 were measured and evaluated for the magnetic tape. Those results Fi table-1
Shown below.
実施例８〜１５
表−５に示すリン酸エステルとカップリング剤を用いて
、実施例１で使用したＣｏ 被着γ−Ｆｅ２０．１５０
１／の表面を実施例７の方法に単じて処理し、処理磁性
粉末、磁性塗料および磁気テープを得た。＃磁気テープ
につき実施例１に示した５項目の測定、評価を行った。Examples 8 to 15 Using the phosphoric acid ester and coupling agent shown in Table 5, Co-adhered γ-Fe20.150 used in Example 1 was prepared.
The surface of 1/1 was simply treated by the method of Example 7 to obtain treated magnetic powder, magnetic paint, and magnetic tape. #The five items shown in Example 1 were measured and evaluated for the magnetic tape.
それらの結果ｒｉ表−１に示す。The results are shown in Table 1.
比較例１
実施例１で用いたＣＯ被着ｒ−Ｆｅ２Ｏ２を何ら表面処
理することなしに、分散剤として大豆油レジチアｆＯｏ
被着ｒ−Ｆｅ２０．１００ Ｍｉｉ部あた）２．４重量
部用いて、以下実施例１の方法に準じて磁性塗料と磁気
テープを得た。該磁気テープにつき実施例１に示した５
項目の測定、評価を行った。それらの結果は表−１に示
す。Comparative Example 1 The CO-adhered r-Fe2O2 used in Example 1 was treated with soybean oil Resitia fOo as a dispersant without any surface treatment.
A magnetic paint and a magnetic tape were obtained according to the method of Example 1 using 2.4 parts by weight of r-Fe (20.100 parts by weight). 5 shown in Example 1 for the magnetic tape.
Items were measured and evaluated. The results are shown in Table-1.
比較例２
比較例１で用いた大豆油レシチンの代わｐにオクチルホ
スフェート２．４重量部を用いる以外は比較例１と同様
の方法によシ磁性塗料及び磁気テープを得た。該磁気テ
ープにつき実施例１に準じて５項目の測定、評価を行っ
た。それらの結果を表−１に示す。Comparative Example 2 A magnetic paint and magnetic tape were obtained in the same manner as in Comparative Example 1, except that 2.4 parts by weight of octyl phosphate was used in place of the soybean oil lecithin used in Comparative Example 1. Five items of measurement and evaluation were performed on the magnetic tape in accordance with Example 1. The results are shown in Table-1.
比較例５
冷却管付５００Ｉｌｌセパラブルフラスコに、実施例１
で用いたＣＯ被着ｒ−Ｆｅ１２． １５０ 、？、）ル
エン５ｏｏｔｉ、有機シラン化合物である（ＣＨ３０）
３ＳＩＣ３Ｈ６ＮＨ０２Ｈ４ＮＨ２を５ｇを入れ７５Ｃ
〜８５Ｃで２時間攪拌した。次いで、過剰のトルエンで
磁性粉を洗浄し、減圧下６０ｔｌ’ＩＣ保ちトルエンを
除去し、上記１機シラン化合物で表面処理された磁性粉
を得た。Comparative Example 5 Example 1 was placed in a 500 Ill separable flask with a cooling tube.
The CO-coated r-Fe12. 150,? ,) Luene 5ooti is an organosilane compound (CH30)
Add 5g of 3SIC3H6NH02H4NH2 and 75C
Stirred at ~85C for 2 hours. Next, the magnetic powder was washed with excess toluene, and the toluene was removed under reduced pressure at 60 tl' IC to obtain magnetic powder surface-treated with the above-mentioned silane compound.
＃磁性粉にセスキドデシルポリオキシエチレン（９モル
付加）ホスフェ−）６．９．および実施例１で用いたバ
インダーと溶削全混合しボールミルで４８時間混練した
後、実施例１で用いた硬化剤を入れて系が均一になるま
で攪拌して磁性塗料？得た。さらに実施例１の方法に準
じて磁気テープを製造し、実施例１に示した５項目の測
定、評価を行った。それらの結果線表−１に示す。#Sesquidodecylpolyoxyethylene (9 mol addition) phosphate to magnetic powder) 6.9. Then, the binder used in Example 1 and the fusing were mixed together and kneaded in a ball mill for 48 hours, then the curing agent used in Example 1 was added and stirred until the system became homogeneous. Obtained. Furthermore, a magnetic tape was manufactured according to the method of Example 1, and the five items shown in Example 1 were measured and evaluated. The results are shown in Table 1.
比較例４
５００１Ｌｔセパラブルフラスコに、実施例１で用いた
Ｃｏ 被着ｒ−Ｆａ２０．１５０１／、トルエン５００
１、および実施例１で用いたリン酸エステル６Ｉを入れ
呈温で２時間攪拌した。その後、減圧下６０Ｃに保ちト
ルエンを除去した。得られた磁性粉につき、以下実施例
１の方法に準じて磁性塗料、磁気テープを得た。＃磁気
テープにつき実施例１に示した５項目の側足、評価を行
った。それらの結果は表−１に示す。Comparative Example 4 A 5001Lt separable flask was coated with Co used in Example 1, r-Fa 20.1501/, toluene 500
1 and phosphoric acid ester 6I used in Example 1 were added and stirred at room temperature for 2 hours. Thereafter, the pressure was kept at 60C to remove toluene. Using the obtained magnetic powder, a magnetic paint and a magnetic tape were obtained according to the method of Example 1. #The side legs of the magnetic tape were evaluated in the five items shown in Example 1. The results are shown in Table-1.
比較例５
実施例１で用いたＣｏ 被着ｒ−Ｆｅ２０３を何ら表面
処理することなしに１分散剤として大豆油レシチンをＣ
ｏ被着ｒ−Ｆｅ５Ｏ１２００電量部あたシ２．４重量部
用いて、以下実施例７の方法に進じて磁性塗料と磁気テ
ープを得た。該磁気テープにつき実施例１に示した５項
目の測定、評価を行った。それらの結果は表−１に示す
。Comparative Example 5 Soybean oil lecithin was added as a dispersant to Co-adhered r-Fe203 used in Example 1 without any surface treatment.
Using 1200 coulometric parts and 2.4 parts by weight of r-Fe5O, the method of Example 7 was followed to obtain a magnetic paint and a magnetic tape. The five items shown in Example 1 were measured and evaluated for the magnetic tape. The results are shown in Table-1.
比較例６
比較例５で用いた大豆油レシチンのかわシにオクチルホ
スフェート２．４電量部を用いる以外は比較例５と同様
の方法により磁性塗料及び磁気テープを得た。該磁気テ
ープにつき実施例１に示した５項目の測定、評価を行っ
た。それらの結果は表−１に示す。Comparative Example 6 A magnetic paint and a magnetic tape were obtained in the same manner as in Comparative Example 5, except that 2.4 parts of octyl phosphate was used in the soybean oil lecithin base used in Comparative Example 5. The five items shown in Example 1 were measured and evaluated for the magnetic tape. The results are shown in Table-1.
表−１ 表−２ （注）東） ・ＫＢＭ−６００００３Ｈ６００００１，Ｈ，。Table-1 Table-2 (Note) East) ・KBM-600003H600001,H,.
０Ｈ３０−Ｓニー（ａｏｏｏ５．Ｈ，）２・プレンアク
トに−４４（ｊＪｉ（ＯＨ３）２０ＴＬｆＯ０２Ｈ４Ｍ
ＨＯ２Ｈ４ＨＨ２）３・ＫＢＭ−４０５実施例１で用い
た有機シラン化合物と同一。0H30-S Knee (aooo5.H,) 2 Plain Act -44 (jJi (OH3) 20TLfO02H4M
HO2H4HH2)3.KBM-405 Same as the organic silane compound used in Example 1.
表−５
（注）リリン酸エステル蒼含有ビニルモノマー（日本化
薬製）
＊＊） ｏＨ（ａｎ ３）２ｏｒｔ（ｏｏｏｃ、、Ｈ３
５） ５実施例１６
冷却管（ｔ４ツロフラスコにトルエン５００ｄ。Table-5 (Note) Vinyl monomer containing phosphoric acid ester (manufactured by Nippon Kayaku) **) oH (an 3) 2 ort (oooc,, H3
5) 5 Example 16 Cooling tube (500 d of toluene in a T4 Tulo flask.
ガス中蒸発法超微粒Ｆｅ−Ｎｉ合金（平均粒径５００Ａ
、Ｈｃ１５０００ａ、σＢ １５０ ｅｍｕ／＃ ）５
０ｐ、シランカップリング剤である
Ｈ２Ｎ０２Ｈ４ＮＨ０５Ｈ６Ｆ３ｉ（００２Ｈ５）、を
ｏ、ａ３オクタデシルポリオキシエチレン（５モル付加
）ホスフェ−）２．Ｆ？ｉ入れ、攪拌しながら？ＤＣで
２時間加熱し、その後冷却して多量のトルエンで洗浄し
て表面処理磁性粉を得た。Ultrafine grained Fe-Ni alloy (average grain size 500A)
, Hc15000a, σB 150 emu/# )5
0p, silane coupling agent H2N02H4NH05H6F3i (002H5), o, a3 octadecyl polyoxyethylene (5 mole addition) phosphate)2. F? Add it while stirring? The mixture was heated with DC for 2 hours, then cooled and washed with a large amount of toluene to obtain surface-treated magnetic powder.
該処理磁性粉末と、バインダーとして実施例７で用いた
ニトロセルに−ス系バインダーとポリウレタン樹脂の１
＝１（重量比）の混合物を磁性粉末九対して４５重量％
及び溶剤としてメチルエチルケトン：シクロへキサノン
：トルエンとの１：ｔ：１（重量比）１００．９を混合
してサンドグラインダーで５時間混練し、さらに硬化網
（日本ポリウレタン工業（株）のコロネートＬ）をバイ
ンダーに対して２０重ｆｉｌ加えてサンドグラインダー
で５０分間混練して磁性塗料を得た。The treated magnetic powder, the nitrocell-based binder used in Example 7 as a binder, and polyurethane resin 1
= 1 (weight ratio) mixture to 45% by weight of magnetic powder 9
and methyl ethyl ketone: cyclohexanone: toluene (1:t:1 (weight ratio) 100.9 as a solvent) were mixed and kneaded for 5 hours using a sand grinder, and then a hardening net (Coronate L from Nippon Polyurethane Industries Co., Ltd.) was mixed. A magnetic coating material was obtained by adding 20 layers of filtrate to the binder and kneading the mixture with a sand grinder for 50 minutes.
次いでこの磁性塗料を５０μｍ のアプリケーターを用
いてポリエステルフィルム上Ｋｍ布し、磁場配向を行わ
ずに熱風乾燥を行い、カレンダー処理して円盤状に打ち
抜き磁気ディスクを得た。Next, this magnetic paint was spread over a polyester film using a 50 μm applicator, dried with hot air without magnetic field orientation, and subjected to calender treatment to be punched out into a disk shape to obtain a magnetic disk.
該磁気ディスクにつき光沢度、残留磁束密度（Ｂｒ入耐
久性（１ｏ００万パス／トラツク後の出力低下）、およ
びＦＲ−ｏｕｔ を測定した。この結果は表−４に示す
。ただし、ＦＲ−ｏｕｔ の測定条件は次のようである
。The glossiness, residual magnetic flux density (Br-input durability (output drop after 1 million passes/track), and FR-out were measured for the magnetic disk. The results are shown in Table 4. However, the FR-out The measurement conditions are as follows.
相対速度； ４．Ｏｒｎ ７秒、記録周波数； ４ Ｍ
Ｈｚ、記録用ヘッド；センダスト、再生用ヘッド；フェ
ライト。Relative velocity; 4. Orn 7 seconds, recording frequency; 4M
Hz, recording head; Sendust, reproduction head; ferrite.
比較例７
実施例１６で用いた超微粉Ｆｅ−Ｎｉ合金５θＩを表面
処理することなしに、分散剤としてリン酸エステル系界
面活性剤を上記超微粉に対して５重量係添加し、以下実
施例１６と同様の方法によシ磁性塗料及び磁気ディスク
を？Ｉｆｃｏ該磁気ディスクにつき、実施例１６と同一
の評価を行った。この結果は表−４に示す。Comparative Example 7 Without surface-treating the ultrafine Fe-Ni alloy 5θI used in Example 16, 5 weight percent of a phosphate ester surfactant was added as a dispersant to the ultrafine powder, and the following examples were prepared. Magnetic paint and magnetic disk using the same method as in 16? The Ifco magnetic disk was evaluated in the same manner as in Example 16. The results are shown in Table-4.
表−４
秦 ＦＲ−ｏｕｔ ｉ；を比較例７の磁気ディスクを０
とする。Table 4 Qin FR-out i; for the magnetic disk of Comparative Example 7
shall be.
Claims (1)
を表わし、Ａは炭素数２〜４のフルキレン基を表わし、
ｎは０又は１〜５０の整数を表し、ｌは１．１．５又は
２を表わす）で表わされるリン酸エステル、および、 値）−分子中圧二個以上のリン酸基’ｌする分子量Ｔ
Ｏ０００以下のリン酸エステル、からなる群より選ばれ
る１穐又は２株以上のリン酸エステルと、 （蜀 −分子中に加水分解性アルコキシシラン基を有す
る有機シラン化合物、 （Ｉｖ）−分子中に加水分解性チタン基を有する有機チ
タン化合物、および、 （ｖ）−分子中に加水分解性アルコキシアルミニウム基
を有する有機アルミニウム化合物。 からなる群よシ選ばれる１種又は２種以上のカップリン
グ剤、 とＫよって表面処理された磁性粉。 ２ 不活性有機溶媒中で、磁性粉を、 （１）次の一般式、 ［ＲＯ（人ｏ ） ｎ］ ｔ Ｐ Ｏ（ＯＨ） ５−１
（式中、Ｒは炭素数２〜２８の炭化水素基又はアシル基
を表わし、ＡＶｉ炭素数２〜４のアルキレン基を表わし
、ｎは０又は１〜５０の整数を表し、ｌは１．１．５又
Ｆｉ２に−表わす）で表わされるリン酸エステル、およ
び。 （１）−分子中に二個以上のリン酸基を有する分子ｔ１
００００以下のリン酸エステル、からなる群よシ選ばれ
る１釉又は２種以上のリン酸エステルと、 （１） −分子中に加水分解性アをコキシシラ７基を有
する有機シラン化合物、 （ロ）−分子中に加水分解性チタン基を有する有機チタ
ン化合物、および。 （ｖ）−分子中に加水分解性アルコキシアルミニウム基
を有する有機アルミニウム化合物、からなる群よ）選ば
れる１種又Ｆｉ２８１以上のカップリンク剤 とを用いて加熱処理を行うことを特徴とする表面処理磁
性粉の製造方法。 五 リン酸エステルおよびカップリング剤を、各々、磁
性粉に対して０．５重量％以上、かつ両者の重量比（リ
ン酸エステル二カップリング剤）が１＝５〜５：１とな
るように使用する特許請求の範囲第２項記載の製造方法
。 ４、 加熱処理温度が６０Ｃ以上である特許請求の範囲
第２項又は第５項記載の製造方法。[Scope of Claims] t(1) The following general formula % formula % (wherein R represents a hydrocarbon group or acyl group having 2 to 28 carbon atoms, and A represents a fullkylene group having 2 to 4 carbon atoms; ,
(n represents 0 or an integer from 1 to 50, l represents 1.1.5 or 2); T
One or more phosphoric esters selected from the group consisting of phosphoric esters having a molecular weight of O000 or less; an organotitanium compound having a hydrolyzable titanium group, and (v) an organoaluminum compound having a hydrolyzable alkoxyaluminum group in the molecule; one or more coupling agents selected from the group consisting of; Magnetic powder surface-treated by K.2 Magnetic powder in an inert organic solvent, (1) The following general formula, [RO(ON)n]t PO(OH) 5-1
(In the formula, R represents a hydrocarbon group or acyl group having 2 to 28 carbon atoms, AVi represents an alkylene group having 2 to 4 carbon atoms, n represents 0 or an integer of 1 to 50, and l is 1.1 .5 or Fi2), and (1) - Molecule t1 having two or more phosphate groups in the molecule
0,000 or less phosphoric esters; (1) - an organosilane compound having 7 hydrolyzable a-koxysila groups in the molecule; (b) - an organic titanium compound having a hydrolyzable titanium group in its molecule; (v) - an organoaluminum compound having a hydrolyzable alkoxyaluminum group in its molecule) or a coupling agent with an Fi of 281 or higher; surface treatment characterized by heat treatment; Method for producing magnetic powder. (v) Phosphate ester and coupling agent are each 0.5% by weight or more based on the magnetic powder, and the weight ratio of both (phosphate ester two coupling agent) is 1 = 5 to 5:1. The manufacturing method according to claim 2 is used. 4. The manufacturing method according to claim 2 or 5, wherein the heat treatment temperature is 60C or higher.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP59085545A JPS60229306A (en) | 1984-04-27 | 1984-04-27 | Surface treatment of magnetic powder and manufacture thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP59085545A JPS60229306A (en) | 1984-04-27 | 1984-04-27 | Surface treatment of magnetic powder and manufacture thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS60229306A true JPS60229306A (en) | 1985-11-14 |
| JPH0334841B2 JPH0334841B2 (en) | 1991-05-24 |
Family
ID=13861822
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP59085545A Granted JPS60229306A (en) | 1984-04-27 | 1984-04-27 | Surface treatment of magnetic powder and manufacture thereof |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS60229306A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5429899A (en) * | 1990-11-19 | 1995-07-04 | Kenrich Petrochemicals, Inc. | Magnetic materials |
| US20100059448A1 (en) * | 2008-09-05 | 2010-03-11 | Kabushiki Kaisha Toshiba | Magnetic particles for water purification and water treatment method employing the same |
-
1984
- 1984-04-27 JP JP59085545A patent/JPS60229306A/en active Granted
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5429899A (en) * | 1990-11-19 | 1995-07-04 | Kenrich Petrochemicals, Inc. | Magnetic materials |
| US20100059448A1 (en) * | 2008-09-05 | 2010-03-11 | Kabushiki Kaisha Toshiba | Magnetic particles for water purification and water treatment method employing the same |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0334841B2 (en) | 1991-05-24 |
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