JPH03278315A - Magnetic recording medium - Google Patents
Magnetic recording mediumInfo
- Publication number
- JPH03278315A JPH03278315A JP7697690A JP7697690A JPH03278315A JP H03278315 A JPH03278315 A JP H03278315A JP 7697690 A JP7697690 A JP 7697690A JP 7697690 A JP7697690 A JP 7697690A JP H03278315 A JPH03278315 A JP H03278315A
- Authority
- JP
- Japan
- Prior art keywords
- magnetic layer
- magnetic
- recording medium
- coating
- magnetic recording
- 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
- 230000005291 magnetic effect Effects 0.000 title claims abstract description 114
- 238000000576 coating method Methods 0.000 claims abstract description 94
- 239000011248 coating agent Substances 0.000 claims abstract description 90
- 239000000843 powder Substances 0.000 claims abstract description 74
- 230000005294 ferromagnetic effect Effects 0.000 claims abstract description 39
- 239000007788 liquid Substances 0.000 claims abstract description 31
- 239000011230 binding agent Substances 0.000 claims abstract description 27
- 229920001228 polyisocyanate Polymers 0.000 claims abstract description 25
- 239000005056 polyisocyanate Substances 0.000 claims abstract description 25
- VPKDCDLSJZCGKE-UHFFFAOYSA-N carbodiimide group Chemical group N=C=N VPKDCDLSJZCGKE-UHFFFAOYSA-N 0.000 claims abstract description 12
- 150000001875 compounds Chemical class 0.000 claims description 61
- 239000000203 mixture Substances 0.000 claims description 30
- 238000002156 mixing Methods 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 30
- 239000006229 carbon black Substances 0.000 abstract description 17
- 238000006243 chemical reaction Methods 0.000 abstract description 12
- IQPQWNKOIGAROB-UHFFFAOYSA-N isocyanate group Chemical group [N-]=C=O IQPQWNKOIGAROB-UHFFFAOYSA-N 0.000 abstract description 9
- 239000002904 solvent Substances 0.000 abstract description 8
- 125000000524 functional group Chemical group 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 2
- 239000010410 layer Substances 0.000 abstract 5
- 239000011247 coating layer Substances 0.000 abstract 1
- -1 abrasive Substances 0.000 description 37
- 239000000243 solution Substances 0.000 description 33
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- 238000000034 method Methods 0.000 description 27
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 19
- 229910052799 carbon Inorganic materials 0.000 description 17
- 239000006185 dispersion Substances 0.000 description 17
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 12
- 235000014113 dietary fatty acids Nutrition 0.000 description 12
- 239000000194 fatty acid Substances 0.000 description 12
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 10
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- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical group OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 8
- 125000004432 carbon atom Chemical group C* 0.000 description 8
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- 239000000956 alloy Substances 0.000 description 7
- RTTZISZSHSCFRH-UHFFFAOYSA-N 1,3-bis(isocyanatomethyl)benzene Chemical compound O=C=NCC1=CC=CC(CN=C=O)=C1 RTTZISZSHSCFRH-UHFFFAOYSA-N 0.000 description 6
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- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 description 6
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 5
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- 239000012298 atmosphere Substances 0.000 description 4
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- 238000004132 cross linking Methods 0.000 description 4
- 150000002148 esters Chemical class 0.000 description 4
- MMKRHZKQPFCLLS-UHFFFAOYSA-N ethyl myristate Chemical compound CCCCCCCCCCCCCC(=O)OCC MMKRHZKQPFCLLS-UHFFFAOYSA-N 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 150000003014 phosphoric acid esters Chemical class 0.000 description 4
- 229920006122 polyamide resin Polymers 0.000 description 4
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- 238000001179 sorption measurement Methods 0.000 description 4
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- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 3
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical group CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 3
- 229920000877 Melamine resin Polymers 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 3
- 235000021355 Stearic acid Nutrition 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 230000002378 acidificating effect Effects 0.000 description 3
- 125000005396 acrylic acid ester group Chemical group 0.000 description 3
- 239000000654 additive Substances 0.000 description 3
- 150000001298 alcohols Chemical class 0.000 description 3
- 125000000217 alkyl group Chemical group 0.000 description 3
- 125000003277 amino group Chemical group 0.000 description 3
- HGAZMNJKRQFZKS-UHFFFAOYSA-N chloroethene;ethenyl acetate Chemical compound ClC=C.CC(=O)OC=C HGAZMNJKRQFZKS-UHFFFAOYSA-N 0.000 description 3
- 239000011651 chromium Substances 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 125000005442 diisocyanate group Chemical group 0.000 description 3
- ZQPPMHVWECSIRJ-MDZDMXLPSA-N elaidic acid Chemical compound CCCCCCCC\C=C\CCCCCCCC(O)=O ZQPPMHVWECSIRJ-MDZDMXLPSA-N 0.000 description 3
- 125000004185 ester group Chemical group 0.000 description 3
- 239000000945 filler Substances 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 3
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 3
- 238000004898 kneading Methods 0.000 description 3
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- 229910052753 mercury Inorganic materials 0.000 description 3
- 125000005397 methacrylic acid ester group Chemical group 0.000 description 3
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 3
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 3
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 3
- 239000003960 organic solvent Substances 0.000 description 3
- 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 3
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- 239000010936 titanium Substances 0.000 description 3
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- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 2
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 2
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 2
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical group OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 description 2
- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 description 2
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
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- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
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- QOSSAOTZNIDXMA-UHFFFAOYSA-N Dicylcohexylcarbodiimide Chemical compound C1CCCCC1N=C=NC1CCCCC1 QOSSAOTZNIDXMA-UHFFFAOYSA-N 0.000 description 2
- ROSDSFDQCJNGOL-UHFFFAOYSA-N Dimethylamine Chemical compound CNC ROSDSFDQCJNGOL-UHFFFAOYSA-N 0.000 description 2
- 229910015189 FeOx Inorganic materials 0.000 description 2
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 2
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- 239000005058 Isophorone diisocyanate Substances 0.000 description 2
- BAVYZALUXZFZLV-UHFFFAOYSA-N Methylamine Chemical compound NC BAVYZALUXZFZLV-UHFFFAOYSA-N 0.000 description 2
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- 150000001413 amino acids Chemical class 0.000 description 2
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- GHVNFZFCNZKVNT-UHFFFAOYSA-N decanoic acid Chemical compound CCCCCCCCCC(O)=O GHVNFZFCNZKVNT-UHFFFAOYSA-N 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
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- ALSTYHKOOCGGFT-KTKRTIGZSA-N (9Z)-octadecen-1-ol Chemical compound CCCCCCCC\C=C/CCCCCCCCO ALSTYHKOOCGGFT-KTKRTIGZSA-N 0.000 description 1
- OYHQOLUKZRVURQ-NTGFUMLPSA-N (9Z,12Z)-9,10,12,13-tetratritiooctadeca-9,12-dienoic acid Chemical compound C(CCCCCCC\C(=C(/C\C(=C(/CCCCC)\[3H])\[3H])\[3H])\[3H])(=O)O OYHQOLUKZRVURQ-NTGFUMLPSA-N 0.000 description 1
- OWQPOVKKUWUEKE-UHFFFAOYSA-N 1,2,3-benzotriazine Chemical compound N1=NN=CC2=CC=CC=C21 OWQPOVKKUWUEKE-UHFFFAOYSA-N 0.000 description 1
- QMMJWQMCMRUYTG-UHFFFAOYSA-N 1,2,4,5-tetrachloro-3-(trifluoromethyl)benzene Chemical compound FC(F)(F)C1=C(Cl)C(Cl)=CC(Cl)=C1Cl QMMJWQMCMRUYTG-UHFFFAOYSA-N 0.000 description 1
- WSLDOOZREJYCGB-UHFFFAOYSA-N 1,2-Dichloroethane Chemical compound ClCCCl WSLDOOZREJYCGB-UHFFFAOYSA-N 0.000 description 1
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 description 1
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- PSXNDMJWRZYVTM-UHFFFAOYSA-N octanoic acid butyl ester Natural products CCCCCCCC(=O)OCCCC PSXNDMJWRZYVTM-UHFFFAOYSA-N 0.000 description 1
- BBZAGOMQOSEWBH-UHFFFAOYSA-N octyl dodecanoate Chemical compound CCCCCCCCCCCC(=O)OCCCCCCCC BBZAGOMQOSEWBH-UHFFFAOYSA-N 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 235000019198 oils Nutrition 0.000 description 1
- 235000021313 oleic acid Nutrition 0.000 description 1
- BARWIPMJPCRCTP-UHFFFAOYSA-N oleic acid oleyl ester Natural products CCCCCCCCC=CCCCCCCCCOC(=O)CCCCCCCC=CCCCCCCCC BARWIPMJPCRCTP-UHFFFAOYSA-N 0.000 description 1
- 229940055577 oleyl alcohol Drugs 0.000 description 1
- XMLQWXUVTXCDDL-UHFFFAOYSA-N oleyl alcohol Natural products CCCCCCC=CCCCCCCCCCCO XMLQWXUVTXCDDL-UHFFFAOYSA-N 0.000 description 1
- BARWIPMJPCRCTP-CLFAGFIQSA-N oleyl oleate Chemical compound CCCCCCCC\C=C/CCCCCCCCOC(=O)CCCCCCC\C=C/CCCCCCCC BARWIPMJPCRCTP-CLFAGFIQSA-N 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 150000003891 oxalate salts Chemical class 0.000 description 1
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 1
- VTRUBDSFZJNXHI-UHFFFAOYSA-N oxoantimony Chemical compound [Sb]=O VTRUBDSFZJNXHI-UHFFFAOYSA-N 0.000 description 1
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- CAQRFUZAAAEILW-UHFFFAOYSA-N oxygen(2-) tin(4+) titanium(4+) Chemical compound [O--].[O--].[O--].[O--].[Ti+4].[Sn+4] CAQRFUZAAAEILW-UHFFFAOYSA-N 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- MOQRZWSWPNIGMP-UHFFFAOYSA-N pentyl octadecanoate Chemical compound CCCCCCCCCCCCCCCCCC(=O)OCCCCC MOQRZWSWPNIGMP-UHFFFAOYSA-N 0.000 description 1
- 239000012169 petroleum derived wax Substances 0.000 description 1
- 235000019381 petroleum wax Nutrition 0.000 description 1
- 239000005011 phenolic resin Substances 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- ACVYVLVWPXVTIT-UHFFFAOYSA-M phosphinate Chemical compound [O-][PH2]=O ACVYVLVWPXVTIT-UHFFFAOYSA-M 0.000 description 1
- 125000005496 phosphonium group Chemical group 0.000 description 1
- 238000009832 plasma treatment Methods 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920000233 poly(alkylene oxides) Polymers 0.000 description 1
- 229920003207 poly(ethylene-2,6-naphthalate) Polymers 0.000 description 1
- 229920002492 poly(sulfone) Polymers 0.000 description 1
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 229920000768 polyamine Polymers 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 229920005906 polyester polyol Polymers 0.000 description 1
- 239000011112 polyethylene naphthalate Substances 0.000 description 1
- 229920000151 polyglycol Polymers 0.000 description 1
- 239000010695 polyglycol Substances 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 239000009719 polyimide resin Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 229920005672 polyolefin resin Polymers 0.000 description 1
- 229920013636 polyphenyl ether polymer Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 229920000915 polyvinyl chloride Polymers 0.000 description 1
- 239000004800 polyvinyl chloride Substances 0.000 description 1
- 239000005033 polyvinylidene chloride Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 150000003242 quaternary ammonium salts Chemical class 0.000 description 1
- 239000001397 quillaja saponaria molina bark Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000007763 reverse roll coating Methods 0.000 description 1
- 229910052702 rhenium Inorganic materials 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000010458 rotten stone Substances 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 229930182490 saponin Natural products 0.000 description 1
- 150000007949 saponins Chemical class 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 229910052706 scandium Inorganic materials 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 229920002050 silicone resin Polymers 0.000 description 1
- 125000005373 siloxane group Chemical group [SiH2](O*)* 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 125000003808 silyl group Chemical group [H][Si]([H])([H])[*] 0.000 description 1
- 239000000344 soap Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000012279 sodium borohydride Substances 0.000 description 1
- 229910000033 sodium borohydride Inorganic materials 0.000 description 1
- 229910001379 sodium hypophosphite Inorganic materials 0.000 description 1
- RPACBEVZENYWOL-XFULWGLBSA-M sodium;(2r)-2-[6-(4-chlorophenoxy)hexyl]oxirane-2-carboxylate Chemical compound [Na+].C=1C=C(Cl)C=CC=1OCCCCCC[C@]1(C(=O)[O-])CO1 RPACBEVZENYWOL-XFULWGLBSA-M 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- 229920003048 styrene butadiene rubber Polymers 0.000 description 1
- 125000001424 substituent group Chemical group 0.000 description 1
- RVEZZJVBDQCTEF-UHFFFAOYSA-N sulfenic acid Chemical group SO RVEZZJVBDQCTEF-UHFFFAOYSA-N 0.000 description 1
- BUUPQKDIAURBJP-UHFFFAOYSA-N sulfinic acid Chemical group OS=O BUUPQKDIAURBJP-UHFFFAOYSA-N 0.000 description 1
- 125000001174 sulfone group Chemical group 0.000 description 1
- RWSOTUBLDIXVET-UHFFFAOYSA-O sulfonium group Chemical group [SH3+] RWSOTUBLDIXVET-UHFFFAOYSA-O 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 229920003051 synthetic elastomer Polymers 0.000 description 1
- 239000005061 synthetic rubber Substances 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- 239000011269 tar Substances 0.000 description 1
- TUNFSRHWOTWDNC-HKGQFRNVSA-N tetradecanoic acid Chemical compound CCCCCCCCCCCCC[14C](O)=O TUNFSRHWOTWDNC-HKGQFRNVSA-N 0.000 description 1
- 125000006337 tetrafluoro ethyl group Chemical group 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 125000003396 thiol group Chemical group [H]S* 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- XTTGYFREQJCEML-UHFFFAOYSA-N tributyl phosphite Chemical compound CCCCOP(OCCCC)OCCCC XTTGYFREQJCEML-UHFFFAOYSA-N 0.000 description 1
- MTPVUVINMAGMJL-UHFFFAOYSA-N trimethyl(1,1,2,2,2-pentafluoroethyl)silane Chemical compound C[Si](C)(C)C(F)(F)C(F)(F)F MTPVUVINMAGMJL-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 description 1
- ITRNXVSDJBHYNJ-UHFFFAOYSA-N tungsten disulfide Chemical compound S=[W]=S ITRNXVSDJBHYNJ-UHFFFAOYSA-N 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
- 229910000859 α-Fe Inorganic materials 0.000 description 1
Abstract
Description
【発明の詳細な説明】
(産業上の利用分野〕
本発明は、非磁性支持体と磁性層、あるいは磁性層およ
びハ・ツク層よりなる磁気記録媒体の改良に関するもの
である。DETAILED DESCRIPTION OF THE INVENTION (Field of Industrial Application) The present invention relates to an improvement in a magnetic recording medium comprising a nonmagnetic support and a magnetic layer, or a magnetic layer and a hack layer.
〔従来の技術とその問題点]
−Cにオーディオ用、ビデオ用、コンピュータ用(ディ
スク、メモリーテープ)等の磁気記録媒体として、強磁
性粉末を結合剤(バインダー)中に分散させた磁性層を
非磁性支持体上に設けた磁気記録媒体が用いられている
。[Prior art and its problems] - C has a magnetic layer in which ferromagnetic powder is dispersed in a binder as a magnetic recording medium for audio, video, computer use (disks, memory tapes), etc. A magnetic recording medium provided on a non-magnetic support is used.
近年、これらの磁気記録媒体は高密度記録が要求され、
強磁性粉末の微粒子化、合金粉末化、高充填化、磁気記
録媒体の超平滑表面化等により信号/雑音の高信号化や
低雑音化が達成されている。In recent years, these magnetic recording media are required to have high density recording.
Higher signal/noise and lower noise have been achieved by making ferromagnetic powder finer, alloy powder, higher filling, and ultra-smooth surface of magnetic recording media.
又、同一時間で高密度記録を行うには磁気記録媒体への
書き込み速度や呼び込み寸度の短縮化が必要で磁気記録
媒体の高速搬送が要求される。この高速搬送適性のため
走行耐久性や帯電特性、ヘット−・クリーニング特性は
不可欠であり、この目的のためカーボン・ブラックやモ
ース硬度が8以上の研磨剤と称されるフィラーが用いら
れ、具体的には米国特許第3630910号、同第38
3341.2号、同第4614685号、同45392
57号、特開昭59−193533号等に開示されてい
る。In addition, in order to perform high-density recording in the same amount of time, it is necessary to shorten the writing speed and read-in size to the magnetic recording medium, and high-speed transport of the magnetic recording medium is required. Running durability, charging characteristics, and head cleaning characteristics are essential for this high-speed conveyance suitability, and for this purpose fillers called carbon black and abrasives with a Mohs hardness of 8 or higher are used. U.S. Pat. No. 3,630,910 and U.S. Pat. No. 38
3341.2, 4614685, 45392
No. 57, JP-A-59-193533, etc.
しかしこれらの技術をもってしてもテープの高速搬送化
に伴う走行耐久性を充分満足することは極めて困難であ
った。この原因は磁気記録媒体のヤング率を大きくする
ことが困難であることと磁性層の表面性を充分に平滑に
できないところに原因している。この理由は非磁性支持
体上に磁性液及び/またはパック液を塗設してなる磁気
記録媒体の結合剤のうち、ポリイソイアネート及び/ま
たはイソイアネートが調整した塗布液中の水分と反応し
、有効な結合剤、樹脂との架橋反応に寄与できなくなる
ためである。この塗布液中の水分を低減すれば有効な架
橋反応を行うことができるが、塗布液中の水分は大半が
原材料の粉末や樹脂、有機溶剤に起因し、さらに塗布液
の製造工程中に大気中からも水分が入り、この塗布液の
水分制御:よ極めて困難であった。本発明者等は、この
塗布液の水分の制御方法を確立し、かつ磁気記録媒体の
ヤング率を大きくすることをの技術を6育立し、走行耐
久性を飛躍的↓こ向上せしめえることにより本発明を考
案するに到った。また本発明の別の目的は磁性層を構成
する粉体を別々に分散し分散効率を上げて磁性層の表面
性を改善し、高S/Nを得ることである。However, even with these techniques, it has been extremely difficult to sufficiently satisfy the running durability associated with high-speed tape conveyance. This is due to the difficulty in increasing the Young's modulus of the magnetic recording medium and the inability to make the surface of the magnetic layer sufficiently smooth. The reason for this is that polyisocyanate and/or isocyanate, which is a binder for magnetic recording media made by coating a magnetic liquid and/or pack liquid on a non-magnetic support, reacts with moisture in the prepared coating liquid. This is because the effective binder cannot contribute to the crosslinking reaction with the resin. An effective crosslinking reaction can be carried out by reducing the water content in the coating solution, but most of the moisture in the coating solution comes from raw material powders, resins, and organic solvents. Moisture entered from inside, making it extremely difficult to control the moisture content of this coating solution. The inventors of the present invention have established a method for controlling the water content of this coating liquid, and have developed a technology for increasing the Young's modulus of magnetic recording media, thereby dramatically improving running durability. As a result, the present invention was devised. Another object of the present invention is to separately disperse the powder constituting the magnetic layer to increase the dispersion efficiency, improve the surface properties of the magnetic layer, and obtain a high S/N.
(発明の目的〕
本発明の目的は、第1乙こ、高い信転性のある走行耐久
性を得ることのできる磁気記録媒体を捉供することにあ
る。第2に、磁性層の表面性を改善じ、高S/Nを得る
ことのできる磁気記録媒体を捉供することにある。(Objective of the Invention) The first object of the present invention is to provide a magnetic recording medium that can obtain running durability with high reliability.Second, it is desirable to improve the surface properties of the magnetic layer. The object of the present invention is to provide a magnetic recording medium that can improve and obtain a high S/N ratio.
〔課題を解決するための手段]
本発明の目的は、強磁性粉末およびバインダーを含む磁
性層塗布液を塗布して非磁性支持体上に磁性層を設けて
なる磁気記録媒体において、該磁性層塗布液は、カルボ
ジイミド基含有化合物か含有せしめられた後、ポリイソ
イアネート化合物が含有せしめられてなるものであるこ
とを特徴とする磁気記録媒体により達成される。[Means for Solving the Problems] An object of the present invention is to provide a magnetic recording medium in which a magnetic layer is provided on a non-magnetic support by coating a magnetic layer coating liquid containing ferromagnetic powder and a binder. This is achieved by a magnetic recording medium characterized in that the coating liquid contains a carbodiimide group-containing compound and then contains a polyisocyanate compound.
又、本発明の好ましい態様は、以下(1)〜(5)の通
りである。Further, preferred embodiments of the present invention are as shown in (1) to (5) below.
(])強磁磁性粉末、バインダー、カーボンブランク1
.研磨剤、潤滑剤を含む磁性層塗布液を塗布して非磁性
支持体上に磁性層を設けてなる磁気記録媒体において、
該磁性層塗布液は、カルボジイミド基含有化合物が含有
せしめられた後、ポリイソイアネート化合物が含有廿し
められてなるものであり、かつポリイソイアネート化合
物が含有せしめられる前の含水率が0〜0.2重量%で
あること。(]) Ferromagnetic powder, binder, carbon blank 1
.. In a magnetic recording medium in which a magnetic layer is provided on a non-magnetic support by applying a magnetic layer coating liquid containing an abrasive and a lubricant,
The magnetic layer coating solution contains a carbodiimide group-containing compound and then contains a polyisocyanate compound, and has a moisture content of 0 before containing the polyisocyanate compound. ~0.2% by weight.
(2)該磁性層が設けられた非磁性支持体面の反対面に
バインダーを含むバック層塗布液を塗布して設けられた
バック層を有し、該バックN塗布液は、カルボジイミ)
・基含有化合物が含有せしめられた後、ポリイソイアネ
ート化合物が含有せしめられてなるものであり、かつポ
リイソイア第一ト化合物が含有セしめら4る前の含水率
が0〜02重量%であること
(3)該非磁性支持体が、ポリエステルからなり、かつ
磁性層及び、/またはバック層を塗設した後、直ち(こ
カレンクー処理を施したこと。(2) A back layer is provided by coating a back layer coating liquid containing a binder on the opposite side of the non-magnetic support surface on which the magnetic layer is provided, and the back N coating liquid is a carbodiimide).
- A polyisocyanate compound is added after the group-containing compound is added, and the water content before the polyisoyanate compound is added is 0 to 02% by weight. (3) The non-magnetic support is made of polyester and is subjected to a coating treatment immediately after the magnetic layer and/or back layer is applied.
(4)該非6ffi性支持体が、ポリエステルからなり
、かつ磁性面皮び/またはハ・7り層を塗設した後、直
ちにカレンダー処理を施し、次いで相対湿度60%以上
の環境下で磁性層及び/またはバック層を硬化せしめた
こと。(4) The non-6ffi support is made of polyester, and after coating the magnetic layer/layer, it is immediately calendered, and then the magnetic layer and layer are coated in an environment with a relative humidity of 60% or more. /or The back layer has been hardened.
(5)組成成分としてカーボンブラ・ツクを分散してな
る該磁性層塗布液用組成物と組成成分として研磨剤を分
散してなる該(、磁性層塗布液用組成物を混合して後、
この混合液にカルボジイミド基含有化合物を添加し、つ
いでポIJイソイアネーl−化合物を添加して調製され
た該磁性層塗布液を磁性層に塗布すること。(5) After mixing the composition for a magnetic layer coating liquid in which carbon black is dispersed as a component and the composition for a magnetic layer coating liquid in which an abrasive is dispersed as a component,
Adding a carbodiimide group-containing compound to this mixed solution, and then adding a poIJ isoyanyl-compound to coat the magnetic layer with the magnetic layer coating solution prepared.
本発明は、カルボジイミド基含有化合物(以下、本発明
の化合物と言う)を使用することにより、塗布液中に存
在する水を本発明の化合物と反応させることにより除去
し、磁性層及びもしくはバック層のバインダーのポリイ
ソイアネート化合物のイソシアフート基の水との反応を
防止することにより、イソシアネート基をバインダーの
官能基と充分に反応せしめて、三次元網目構造を形成す
る塗膜の硬化反応を効率よく進行せしめ、磁気記録媒体
のヤング率を高くし耐久性を著しく向上せしめるもので
ある。The present invention uses a carbodiimide group-containing compound (hereinafter referred to as the compound of the present invention) to remove water present in the coating solution by reacting with the compound of the present invention, and removes water from the magnetic layer and/or back layer. By preventing the isocyanate group of the polyisocyanate compound of the binder from reacting with water, the isocyanate group is sufficiently reacted with the functional group of the binder, and the curing reaction of the coating film that forms a three-dimensional network structure is activated. This allows for efficient progress, increases the Young's modulus of the magnetic recording medium, and significantly improves the durability.
また、本発明の磁気記録媒体は、磁性層塗布液の調製に
おいて上記のように磁性層の強磁性粉末、およびそれと
と共に添加されるカーボンブラック、研磨剤等の無機粉
体を種類別に別個に溶剤に分散することにより、無機粉
体の分散性が向上すると共に効果的な水分除去が行われ
るため磁性層の膜強化と共に表面性をも改善し高S 、
/ Nを得ることができる。Further, in the magnetic recording medium of the present invention, in preparing the magnetic layer coating solution, the ferromagnetic powder of the magnetic layer and the inorganic powders such as carbon black and abrasives added together with the ferromagnetic powder are separately prepared by solvent. By dispersing the inorganic powder into the powder, the dispersibility of the inorganic powder is improved, and water is effectively removed, which strengthens the magnetic layer and improves the surface properties.
/N can be obtained.
これは、粉体の種類によって、分散が飽和に達する時間
に差があるためと推察される。即ち、従来、例えば、強
磁性粉末、研磨剤、カーボンブラックを同時に分散して
きたが、その結果、強磁性粉末が早く分散され、研磨剤
、カーホンブラックの順となり各々の粉体の分散レベル
は異なったものであり理想的な分散状態に調整すること
が困難であったと考えられる。従って、各々の粉体を別
分散することにより分散度が飽和している組成液が得ら
れ、これらを混和することにより、各々の粉体の分散性
を改善できたものと推察される。This is presumably because the time for dispersion to reach saturation differs depending on the type of powder. That is, conventionally, for example, ferromagnetic powder, abrasive, and carbon black have been dispersed at the same time, but as a result, the ferromagnetic powder is dispersed quickly, followed by the abrasive, and then carbon black, and the dispersion level of each powder is low. It is thought that it was difficult to adjust to the ideal dispersion state because the particles were different. Therefore, it is presumed that by separately dispersing each powder, a composition liquid with saturated dispersion was obtained, and by mixing these, the dispersibility of each powder could be improved.
本発明の化合物を用いることにより、磁性層塗布液及び
バック層塗布液のポリイソイアネート化合物添加以前の
含水率を好ましくは、0〜0.2重量%に制御すること
により磁性層およびバック層の塗布膜のヤング率を高め
るものであるが、この範囲に制御しないとポリイソシア
2−ト化合物やイソシアネート基を少なくとも有する樹
脂等のイソシアネートMと塗布液中の水が反応し有効な
架橋硬化反応に寄与せずヤング率の低下が生じる。By using the compound of the present invention, the water content of the magnetic layer coating solution and the back layer coating solution before addition of the polyisocyanate compound is preferably controlled to 0 to 0.2% by weight, thereby forming the magnetic layer and the back layer. However, if the Young's modulus of the coating film is not controlled within this range, the isocyanate M such as a polyisocyanate compound or a resin having at least an isocyanate group will react with water in the coating solution, resulting in an effective crosslinking and curing reaction. There is no contribution and the Young's modulus decreases.
更に、該イソシアネート基が水と反応すると炭酸ガスが
発生し、塗布膜にピンホール欠陥が生じて好ましくない
。この塗布液中の水分の源は、主に塗布液を構成する原
材料、及び塗布液製造中における大気中からの水分であ
る。特に塗布液を構成する原材料、即ち、組成成分の強
磁性粉末、バインダー、カーボンブランク、研磨剤等に
は水分が通常、0.2〜5重量%含まれており、塗布液
中の水分を制御することは、従来極めて困難であった技
術である。Furthermore, when the isocyanate group reacts with water, carbon dioxide gas is generated, which is undesirable because pinhole defects occur in the coating film. The sources of moisture in this coating liquid are mainly raw materials constituting the coating liquid and moisture from the atmosphere during manufacturing of the coating liquid. In particular, the raw materials that make up the coating solution, i.e., the compositional components such as ferromagnetic powder, binder, carbon blank, abrasive, etc., usually contain 0.2 to 5% by weight of water, and the moisture content in the coating solution is controlled. This is a technique that has traditionally been extremely difficult.
磁性層塗布液、バック層塗布液の含水率を効果的に低減
せしめる具体的な手段は、本発明の化合物をポリイソイ
アネート化合物の添加に先立ってポリイソイアネート化
合物を含有しない組成成分からなる磁性層塗布液用組成
物に添加して、組成成分に起因する水分を本発明の化合
物と反応せしめて除去することにより塗布液含水率を0
〜0゜2重量%に制御した後、該ポリイソイアネート化
合物を添加する方法が挙げられる。A specific means for effectively reducing the water content of the magnetic layer coating solution and the back layer coating solution is to remove the compound of the present invention from the composition containing no polyisocyanate compound before adding the polyisocyanate compound. The water content of the coating liquid can be reduced to 0 by adding it to the composition for a magnetic layer coating liquid and reacting with the compound of the present invention to remove water caused by the composition components.
An example of a method is to add the polyisocyanate compound after controlling the amount to 0.2% by weight.
この場合、本発明の化合物の添加時期は、ポリイソイア
ネート化合物を添加する時点の塗布液の含水率が上記範
囲であれば特に限定されず、−度に添加しても、分割し
て添加しても任意であるが、好ましくは、強磁性粉末、
研磨剤、等の無機粉体をバインダーおよび溶剤と共に分
散して後添加することが本発明の化合物と水との反応を
効果的に促進するうえで望ましい。特に、無機粉体を比
較的多量に使用する場合、それらを機能別に別個に樹脂
と共に分散して磁性層塗布液用組成物、バック層塗布液
用組成物を調製後、本発明の化合物を添加し、好ましく
は、10分〜48時間、15乃至40°Cの条件で塗布
液中の水と反応させることが好ましい。。In this case, the timing of adding the compound of the present invention is not particularly limited as long as the water content of the coating solution at the time of adding the polyisocyanate compound is within the above range. ferromagnetic powder is optional, but preferably ferromagnetic powder,
In order to effectively promote the reaction between the compound of the present invention and water, it is desirable to disperse an inorganic powder such as an abrasive together with a binder and a solvent and add it later. In particular, when a relatively large amount of inorganic powder is used, the compound of the present invention is added after dispersing the inorganic powders with the resin separately according to their functions to prepare a composition for the magnetic layer coating solution and a composition for the back layer coating solution. However, it is preferable to react with water in the coating liquid under conditions of 15 to 40°C for 10 minutes to 48 hours. .
この場合、磁性層塗布液用組成物、バック層塗布液用組
成物への本発明の化合物(本発明の化合物自体が磁性層
塗布液用組成物とも言える。)の添加は、組成物を混合
した後でも、混合する前でもあるいはそれら両者でも良
いが、通常、混合後が好ましい。In this case, the addition of the compound of the present invention (the compound of the present invention itself can also be said to be a composition for magnetic layer coating solution) to the composition for magnetic layer coating solution and the composition for back layer coating solution involves mixing the compositions. It may be done after mixing, before mixing, or both, but usually after mixing is preferable.
また、これら組成物に起因する塗布液中の水分は上述の
方法により低減でき、また大気中から入る水分に関して
は、製造工程を密閉化して大気中の水分を遮断すること
により実現できる。また、製造工程を密閉化できない場
合は製造工程の設備内を乾燥気体(空気、窒素等)によ
りパージすることにより大気中の水分を遮断することが
できる。Further, the moisture in the coating liquid caused by these compositions can be reduced by the above-mentioned method, and moisture entering from the atmosphere can be reduced by sealing the manufacturing process to block moisture from the atmosphere. Furthermore, if the manufacturing process cannot be sealed, moisture in the atmosphere can be blocked by purging the inside of the equipment for the manufacturing process with dry gas (air, nitrogen, etc.).
本発明の化合物は、下記の通りカルボジイミド基(−N
=C−N−)を含有する化合物(T)であって、N20
と反応するものであれば特に限定されない。The compound of the present invention has a carbodiimide group (-N
=C-N-), the compound (T) contains N20
It is not particularly limited as long as it reacts with.
R’−N=C=N−R” + N20 →
R’−NH−CO−NH−R2(1)
上記一般式(1)中、R1、R2は、同一でも異なって
もよく、上記反応の進行を阻害しない基から選択され、
例えば、炭素数1〜40の炭化水素基、例えば、ジプロ
ピルカルボジイミド、ジーP−トルオイルジイミド等で
互変異性のシアナミドであってもよい。R1,RZは、
好ましくは、炭素数6〜J2の脂環式炭化水素基、特に
好ましくは、下記一般式(II)で表されるジシクロへ
キシルカルボジイミド、及びその誘導体である。R'-N=C=N-R" + N20 →
R'-NH-CO-NH-R2 (1) In the above general formula (1), R1 and R2 may be the same or different and are selected from groups that do not inhibit the progress of the above reaction,
For example, it may be a tautomeric cyanamide with a hydrocarbon group having 1 to 40 carbon atoms, such as dipropylcarbodiimide, di-P-toluoyldiimide, and the like. R1, RZ are
Preferably, it is an alicyclic hydrocarbon group having 6 to J2 carbon atoms, particularly preferably dicyclohexylcarbodiimide represented by the following general formula (II), and derivatives thereof.
R3−C6)+1 o−N−C−N−CJ+ o−R’
(11)上記一般式(11)中、R3、R“
は、水素原子、炭素数20以下の直鎖あるいは分岐のア
ルキル基、アルコキシ基、ハロゲン基、スルフォン基等
を表すが、好ましくは、水素、−CN 、−NO2等の
電子吸引性基が挙げられる。R3-C6)+1 o-N-C-N-CJ+ o-R'
(11) In the above general formula (11), R3, R“
represents a hydrogen atom, a linear or branched alkyl group having 20 or less carbon atoms, an alkoxy group, a halogen group, a sulfone group, etc., and preferably hydrogen, electron-withdrawing groups such as -CN, -NO2, etc. .
本発明の化合物の製造方法等:ま、ンユミノト(Sch
midt)、 et al、 ヘリヒテ(Ber、)
71.1933(1933)、米国特許第265638
3号を参考Q二できる。Method for producing the compound of the present invention, etc.: Ma-Nyuminoto (Sch
midt), et al, Herichte (Ber,)
71.1933 (1933), U.S. Patent No. 265638
I can refer to No.3 Q2.
本発明の化合物は、結合剤総量の2重量%以下添加せし
めることが好ましい。本発明の化合物の塗布液への添加
時期は、ポリイソイアネート化合物を添加する以前であ
るが、ポリイソイアネート化合物を添加した後において
も、更に、本発明の化合物を塗布液に添加することを妨
げるものではない。The compound of the present invention is preferably added in an amount of 2% by weight or less based on the total amount of the binder. The compound of the present invention is added to the coating solution before the polyisocyanate compound is added, but the compound of the present invention may be added to the coating solution even after the polyisocyanate compound is added. It does not prevent this.
又、本発明の化合物は、従来公知の水分除去剤、例えば
、シアノアクリレート、シリカゲル、無水炭酸ナトリウ
ム、塩化カルシウム等と併用することができる。フィラ
ーは工程内↓=設置されたフィルターで除去する。Furthermore, the compound of the present invention can be used in combination with conventionally known water removing agents such as cyanoacrylate, silica gel, anhydrous sodium carbonate, calcium chloride, and the like. Filler is removed in the process ↓ = by the installed filter.
又、本発明の化合物は、磁性層あるいはバック層を設け
た後、そのまま、あるいは適当な溶剤に溶解した後、公
知の塗布手段で本発明の化合物を各層表面から含浸させ
ることができる。この場合の含浸とは、本発明の化合物
を層表面に接触させることにより、本発明の化合物及び
/またはその誘導体(例えば、水との反応生成物)を層
内部及び/または層表面に存在せしめることを言う。Further, after providing the magnetic layer or back layer, the compound of the present invention can be impregnated from the surface of each layer by a known coating method, either as is or after being dissolved in a suitable solvent. Impregnation in this case refers to bringing the compound of the present invention into contact with the layer surface so that the compound of the present invention and/or its derivative (for example, a reaction product with water) is present inside the layer and/or on the layer surface. say something
本発明に使用する強磁性粉末としては、特に、制限はな
く、金属酸化物系、例えば、T−Fe201、Co含有
(被着、変成、ドープ)のT−Fe203、Fe30a
、Co含有(被着、変成、ドープ)のFe、Oa 、
FeOx、Co含有(被着、変成、ドープ)のFeOx
(X=1.33〜1.50)、Cry、やRn、Te
、Sb、Sr、Fe、Ti、V、Mn1、CrzO,、
の少なくとも一種類を含むCry、等、合金あるいは金
属単体系、例えば、金属分が75重量%以上であり、そ
して金属分の60重量%以上が少なくとも1種類の強磁
性金属あるいは合金(例、Fe、Co、Ni、Fe−C
o、Fe−Ni、Co−Ni、C。The ferromagnetic powder used in the present invention is not particularly limited, and metal oxide powders such as T-Fe201, Co-containing (deposited, metamorphosed, doped) T-Fe203, Fe30a
, Co-containing (adhered, modified, doped) Fe, Oa,
FeOx, Co-containing (adhered, metamorphosed, doped) FeOx
(X=1.33~1.50), Cry, Rn, Te
, Sb, Sr, Fe, Ti, V, Mn1, CrzO,,
An alloy or single metal system, such as Cry, containing at least one type of , Co, Ni, Fe-C
o, Fe-Ni, Co-Ni, C.
Ni−Fe、、Co−N1−P、Co−Ni −Fe−
B、Fe−Ni−Zn、Fe−Co−Cr )であり、
該金属分の20重量%以下の範囲内で他の成分(例、A
1、Si、S、Sc、Ti、V、Cr、Mn、Cu、Z
n、Y、Mo、Rh、Pd、Ag、Sn、Sb、Te、
Ba、Ta、W、Re、Au、Hg、Pb、、Bi、L
a、Ce、、Pr、Nd、B、P)を含むことのある合
金等、その他の金属系、例えば、窒化鉄、あるいは合金
系に少量の水、水酸化物または酸化物を含むもの等、更
に、これら系の混合系が挙げられる。Ni-Fe, , Co-N1-P, Co-Ni -Fe-
B, Fe-Ni-Zn, Fe-Co-Cr),
Other components (e.g. A
1, Si, S, Sc, Ti, V, Cr, Mn, Cu, Z
n, Y, Mo, Rh, Pd, Ag, Sn, Sb, Te,
Ba, Ta, W, Re, Au, Hg, Pb, Bi, L
Other metal systems, such as alloys that may contain a, Ce, Pr, Nd, B, P), such as iron nitride, or alloy systems containing small amounts of water, hydroxides or oxides, etc. Further examples include mixed systems of these systems.
これら強磁性粉末の粒子サイズは約0.005〜1sl
の長さで、軸長/細幅の比は、1/1〜50/1程度で
ある。又、これらの強磁性粉末の比表面積は、1%/g
〜70 rd / g程度である。これらの強磁性粉末
の含水率は、0,2〜2.OwL%が好ましいが、本発
明は、本発明の化合物を用いることにより、含水率に対
し、品位の劣る強磁性粉末を使用できるという利点もあ
る。これらの強磁性粉末の表面に、後に述べる分散剤、
潤滑剤、帯電防止剤等をそれぞれの目的の為に分散に先
だって溶剤中で含浸させて、吸着させてもよい。The particle size of these ferromagnetic powders is approximately 0.005 to 1 sl
The ratio of axial length/narrow width is approximately 1/1 to 50/1. In addition, the specific surface area of these ferromagnetic powders is 1%/g
~70rd/g. The moisture content of these ferromagnetic powders is between 0.2 and 2. Although OwL% is preferred, the present invention also has the advantage that by using the compound of the present invention, ferromagnetic powders of inferior quality relative to water content can be used. A dispersant, which will be described later, is applied to the surface of these ferromagnetic powders.
A lubricant, an antistatic agent, etc. may be impregnated in a solvent and adsorbed for each purpose prior to dispersion.
これらの強磁性粉末は、1wt%以内てSr、PbMn
、Ni、Cd、Cr、AI、Si、Ti、Cu、Zn等
の重金属を含む事が好ましい。これらの強磁性粉末にア
ルミナ等を被着、熔融させてもよい。These ferromagnetic powders contain Sr, PbMn within 1wt%
, Ni, Cd, Cr, AI, Si, Ti, Cu, Zn, and other heavy metals. Alumina or the like may be applied to these ferromagnetic powders and melted.
また本発明に使用する強磁性粉末としては、板状六方晶
のバリウムフェライトも使用できる。バリウムフェライ
トの粒子サイズは約0.001〜1ミクロンの直径で厚
みが直径の1/2〜1/20である。バリウムフェライ
トの比重は4〜6g/ccで、比表面積は1ボ/g〜7
0rrf/gである。これらの強磁性粉末の表面には後
で述べる分散剤、潤滑剤、帯電防止剤等をそれぞれの目
的の為に分散に先立って溶剤中で含浸させて、吸着させ
てもよい。Further, as the ferromagnetic powder used in the present invention, plate-shaped hexagonal barium ferrite can also be used. The particle size of barium ferrite is about 0.001 to 1 micron in diameter, and the thickness is 1/2 to 1/20 of the diameter. The specific gravity of barium ferrite is 4 to 6 g/cc, and the specific surface area is 1 bo/g to 7.
It is 0rrf/g. The surface of these ferromagnetic powders may be impregnated with a dispersant, a lubricant, an antistatic agent, etc., which will be described later, in a solvent prior to dispersion for each purpose, and may be adsorbed thereon.
特に、本発明において、強磁性粉末として用いられる強
磁性合金粉末の製造方法の例としては、下記の方法を挙
げることができる。In particular, in the present invention, the following method can be mentioned as an example of a method for manufacturing the ferromagnetic alloy powder used as the ferromagnetic powder.
(a)複合有機酸塩(主としてシュウ酸塩)を水素など
の還元性気体で還元する方法:
(b)酸化鉄を水素などの還元性気体で還元してFeあ
るいはFe−Co粒子などを得る方法:
(c)金属カルボニル化合物を熱分解する方法:(d)
強磁性金属の水溶液に水素化ホウ素ナトリウム、次亜リ
ン酸塩あるいはヒドラジンなどの還元剤を添加して還元
する方法:
(e)水銀陰極を用い強磁性金属粉末を電解析出させた
のち水銀と分離する方法:
(f)金属を低圧の不活性気体中で蒸発させて微粉末を
得る方法:
強磁性合金粉末を使用する場合に、その形状にとくに制
限はないが通常は針状、粒状、サイコロ状、米粒状およ
び板状のものが使用される。この強磁性合金粉末の比表
面積(S[lEア)は35rrr/g以上、好ましくは
、40ボ/g以上、更に好ましくは、45ボ/g以上で
ある。(a) Method of reducing complex organic acid salts (mainly oxalates) with a reducing gas such as hydrogen: (b) Obtaining Fe or Fe-Co particles by reducing iron oxide with a reducing gas such as hydrogen Method: (c) Method of thermally decomposing a metal carbonyl compound: (d)
A method of reducing an aqueous solution of ferromagnetic metal by adding a reducing agent such as sodium borohydride, hypophosphite, or hydrazine: (e) After electrolytically depositing ferromagnetic metal powder using a mercury cathode, mercury and Separation method: (f) Method of obtaining fine powder by evaporating the metal in a low-pressure inert gas: When using ferromagnetic alloy powder, there is no particular restriction on its shape, but it is usually acicular, granular, or Dice-shaped, rice grain-shaped and plate-shaped ones are used. The specific surface area (S[lEa) of this ferromagnetic alloy powder is 35 rrr/g or more, preferably 40 bo/g or more, and more preferably 45 bo/g or more.
本発明の磁性層あるいは更に所望により設けられるバッ
ク層に使用されるバインダーとしては従来公知の熱可塑
性樹脂、熱硬化性樹脂、反応型樹脂やこれらの混合物が
使用される。As the binder used in the magnetic layer of the present invention or the optional back layer, there may be used conventionally known thermoplastic resins, thermosetting resins, reactive resins, and mixtures thereof.
熱可塑性樹脂としては軟化温度が150°C以下、平均
分子量が10000〜300000、重合度が約50〜
2000程度のもので、例えば塩化ビニル酢酸ビニル共
重合体、塩化ビニル重合体、塩化ビニル塩化ビニリデン
共重合体、塩化ビニルアクリロニトリル共重合体、アク
リル酸エステルアクリロニトリル共重合体、アクリル酸
エステル塩化ビニリデン共重合体、アクリル酸エステル
スチレン共重合体、メタクリル酸エステルアクリロニト
リル共重合体、メタクリル酸エステル塩化ビニリデン共
重合体、メタクリル酸エステルスチレン共重合体、ウレ
タンエラストマー、ナイロン−シリコン系樹脂、ニトロ
セルロース−ポリアミド樹脂、ポリフンカビニル、塩化
ビニリデンアクリロニトリル共重合体、ブタジェンアク
リロニトリル共重合体、ポリアミド樹脂、ポリビニルブ
チラール、セルロース誘導体(セルロースアセテートブ
チレーI・、セルロースダイアセテート、セルロースト
リアセテート、セルロースプロピオネート、ニトロセル
ロース、エチルセルロース、メチルセルロース、プロピ
ルセルロース、メチルエチルセルロース、カルボキシメ
チルセルロース、アセチルセルロース等)、スチレンブ
タジェン共重合体、ポリエステル樹脂、り四ロビニルエ
ーテルアクリル酸エステル共重合体、アミノ樹脂、各種
の合成ゴム系の熱可塑性樹脂及びこれらの混合物等が使
用される。The thermoplastic resin has a softening temperature of 150°C or less, an average molecular weight of 10,000 to 300,000, and a degree of polymerization of about 50 to 300,000.
For example, vinyl chloride vinyl acetate copolymer, vinyl chloride polymer, vinyl chloride vinylidene chloride copolymer, vinyl chloride acrylonitrile copolymer, acrylic acid ester acrylonitrile copolymer, acrylic acid ester vinylidene chloride copolymer. combination, acrylic acid ester styrene copolymer, methacrylic acid ester acrylonitrile copolymer, methacrylic acid ester vinylidene chloride copolymer, methacrylic acid ester styrene copolymer, urethane elastomer, nylon-silicon resin, nitrocellulose-polyamide resin, Polyfuncabinyl, vinylidene chloride acrylonitrile copolymer, butadiene acrylonitrile copolymer, polyamide resin, polyvinyl butyral, cellulose derivative (cellulose acetate butyrate I, cellulose diacetate, cellulose triacetate, cellulose propionate, nitrocellulose, ethyl cellulose) , methylcellulose, propylcellulose, methylethylcellulose, carboxymethylcellulose, acetylcellulose, etc.), styrene-butadiene copolymers, polyester resins, tetrarovinyl ether acrylate copolymers, amino resins, various synthetic rubber-based thermoplastic resins and mixtures thereof are used.
熱硬化性樹脂又は反応型樹脂としては塗布液の状態では
200000以下の分子量であり、塗布、乾燥後に加熱
することにより、縮合、付加等の反応により分子量は無
限大のものとなる。又、これらの樹脂のなかで、樹脂が
熱分解するまでの間に軟化又は熔融しないものが好まし
い。具体的には例えばフェノール樹脂、フェノキシ樹脂
、エポキシ樹脂、ポリウレタン硬化型樹脂、尿素樹脂、
メラミン樹脂、アルキッド樹脂、シリコン樹脂、アクリ
ル系反応樹脂、エポキシ−ポリアミド樹脂、ニトロセル
ロースメラミン樹脂、高分子量ポリエステル樹脂とイソ
シアネートプレポリマーの混合物、メタクリル酸塩共重
合体とジイソシアネートプレポリマーの混合物、ポリエ
ステルポリオールとポリイソシアネートとの混合物、尿
素ホルムアルデヒド樹脂、低分子量グリコール/高分子
量ジオール/トリフェニルメタントリイソシアネートの
混合物、ポリアミン樹脂、ポリイミン樹脂及びこれらの
混合物等である。The thermosetting resin or reactive resin has a molecular weight of 200,000 or less in the state of a coating liquid, and when heated after coating and drying, the molecular weight becomes infinite due to reactions such as condensation and addition. Also, among these resins, those that do not soften or melt before the resin is thermally decomposed are preferred. Specifically, for example, phenol resin, phenoxy resin, epoxy resin, polyurethane curable resin, urea resin,
Melamine resins, alkyd resins, silicone resins, acrylic reactive resins, epoxy-polyamide resins, nitrocellulose melamine resins, mixtures of high molecular weight polyester resins and isocyanate prepolymers, mixtures of methacrylate copolymers and diisocyanate prepolymers, polyester polyols and polyisocyanate, urea formaldehyde resin, mixture of low molecular weight glycol/high molecular weight diol/triphenylmethane triisocyanate, polyamine resin, polyimine resin, and mixtures thereof.
これらの熱可塑性樹脂、熱硬化性樹脂、反応型樹脂は、
主たる官能基以外に官能基としてカルボン酸、スルフィ
ン酸、スルフェン酸、スルホン酸、燐酸、硫酸、ポスホ
ン、ホスフィン、ホウ酸、硫酸エステル基、燐酸エステ
ル基、これらのアルキルエステル基等の酸性基(これら
の酸性基は、Na塩などの形でもよい);アミノ酸類、
アミノスルホン酸類、アミノアルコールの硫酸または燐
酸エステル類、アルキルヘタイン型等の両性類基、アミ
ノ基、イミノ基、イミド基、アミド基、エポキシ基、等
また、水酸基、アルコキシル基、チオール基、ハロゲン
基、シリル基、シロキサン基を通常1種以上6種以内含
み、各々の官能基は樹脂1gあたりlXl0−6eq〜
lXl0−2eq含む事が好ましい。These thermoplastic resins, thermosetting resins, and reactive resins are
In addition to the main functional groups, acidic groups such as carboxylic acid, sulfinic acid, sulfenic acid, sulfonic acid, phosphoric acid, sulfuric acid, phosphine, phosphine, boric acid, sulfuric acid ester group, phosphoric ester group, and alkyl ester groups thereof (these The acidic group may be in the form of Na salt, etc.); Amino acids,
Aminosulfonic acids, sulfuric or phosphoric acid esters of aminoalcohols, amphoteric groups such as alkylhetaines, amino groups, imino groups, imido groups, amide groups, epoxy groups, etc. Also, hydroxyl groups, alkoxyl groups, thiol groups, halogens It usually contains one to six types of groups, silyl groups, and siloxane groups, and each functional group contains 1Xl0-6eq to 1g of resin.
It is preferable to include lXl0-2eq.
これらの結合剤の単独又は組合わされたものが使われ、
ほかに添加剤が加えられる。磁性層の強磁性粉末と結合
剤との混合割合は重量比で強磁性粉末100重量部に対
して結合剤5〜300重量部の範囲で使用される。ハ、
り層の粉末と結合剤の混合割合は重量比で粉末100重
量部に対して結合剤30〜300重量部の範囲で使用さ
れる。These binders may be used alone or in combination;
Other additives may be added. The mixing ratio of the ferromagnetic powder and the binder in the magnetic layer is in the range of 5 to 300 parts by weight per 100 parts by weight of the ferromagnetic powder. Ha,
The mixing ratio of the powder and binder for the layer is in the range of 30 to 300 parts by weight based on 100 parts by weight of the powder.
添加剤は分散剤、潤滑剤、研磨剤、帯電防止剤、酸化防
止剤、溶剤等がくわえられる。Additives include dispersants, lubricants, abrasives, antistatic agents, antioxidants, solvents, and the like.
本発明にもちいるポリイソシアネート化合物としては、
イソシアネート基を1分子中に2以上有する化合物であ
れば、特に限定されることはなく、例示すれば、l・リ
レンジイソシア不−1・、4,4ジフエニルメタンジイ
ソシアネート、ヘキサメチレンジイソシアネート、キシ
リレンジイソシア2−ト、ナフチレン−1,5−ジイソ
シアネート、0−トルイジンジイソシア不一ト、イソホ
ロンジイソシアネート、トリフェニルメタントリイソン
アネート、イソホロンジイソシアネート等のイソシア2
−ト類、又当該イソシア7−ト類とボッアルコールとの
生成物、又イソシアネート類の縮合に依って生成した2
〜15量体のポリイソシア不−1・等を使用することが
できる。こ羽らボiJイソシアネート類の平均分子量は
、100〜20000のものが好適である。これらポリ
イソノアネート化合物の市販されている商品名としては
、コロぶ−)L、コロネートHL、コロネート2030
、コロネート2031、ミリオネー) M R、ミリオ
ネートMTL (日本ポリウレタン■製)、タケネー
トD−1,02、タケネートD−11ON、タケネート
D−200、タケネートD−202、タケネート300
S、タケネート500 (武田薬品■製)、スミジュー
ルT−80、スミジュール44S、スミジュールPF、
スミジュールし、スミジュールN、デスモジュールし、
デスモジュールIL、デスモジュールN1デスモジュー
ルHL。The polyisocyanate compounds used in the present invention include:
There are no particular limitations on the compound as long as it has two or more isocyanate groups in one molecule. Examples include 1-lylene diisocyanate, 4,4-diphenylmethane diisocyanate, hexamethylene diisocyanate, and xylene diisocyanate. Isocyanate such as diisocyanate, naphthylene-1,5-diisocyanate, 0-toluidine diisocyanate, isophorone diisocyanate, triphenylmethane trisonanate, isophorone diisocyanate, etc.
-7-ts, products of the isocyanates and botanic alcohol, and 2-2s produced by condensation of isocyanates.
-15-mer polyisocyanate, etc. can be used. The average molecular weight of Kobarabo iJ isocyanates is preferably 100 to 20,000. Commercially available trade names of these polyisonoanate compounds include Corobu-)L, Coronate HL, and Coronate 2030.
, Coronate 2031, Millione) MR, Millionate MTL (manufactured by Nippon Polyurethane), Takenate D-1,02, Takenate D-11ON, Takenate D-200, Takenate D-202, Takenate 300
S, Takenate 500 (manufactured by Takeda Pharmaceutical ■), Sumidur T-80, Sumidur 44S, Sumidur PF,
Sumidur, Sumidur N, Desmodule,
Death module IL, death module N1 death module HL.
デスモジュールT65、デスモジュール15、デスモジ
ュールR、デスモジュールRF、デスモジュールSL、
デスモジュール24273 (住人バイエル社製)等が
あり、これらを単独若しくは硬化反応性の差を利用して
二つ若しくはそハ以上の組み合わせによって使用するこ
とができる。又、硬化反応を促進する目的で、水酸基(
ブタン、・・オール、ヘキサンジオール、分子量が10
00〜1ooooのボリウレクン、水 等)、アミノ基
(モノメチルアミン、ジメチルアミン、l・ジメチルア
ミン等)を有する化合物や金属酸化物の触媒を併用する
事も出来る。これらの水酸基やアミノ基を有する化合物
は多官能である事が望ましい。Desmodule T65, Desmodule 15, Desmodule R, Desmodule RF, Desmodule SL,
There are products such as Desmodur 24273 (manufactured by Sumitomo Bayer), and these can be used alone or in combination of two or more by taking advantage of the difference in curing reactivity. In addition, for the purpose of promoting the curing reaction, hydroxyl groups (
Butane,...ol, hexanediol, molecular weight is 10
It is also possible to use a catalyst of a compound having an amino group (monomethylamine, dimethylamine, l-dimethylamine, etc.) or a metal oxide. It is desirable that these compounds having a hydroxyl group or an amino group are polyfunctional.
これらのポリイソシア7−1・はバインダー総足の5〜
40wt%で用いることが好ましい。These polyisocyas 7-1.
It is preferable to use it at 40 wt%.
また、米国特許公報4596739号に開示されている
ようなケトオキシムフ′ロック型ポリイソノアネートを
用いてもよい。Ketoxime flock polyisonoanates such as those disclosed in US Pat. No. 4,596,739 may also be used.
本発明に使用する分散剤としては、カプリル酸、カプリ
ン酸、ラウリン酸、ミリスチン酸、パルミチン酸、ステ
アリン酸、ベヘン酸、オレイン酸、エライジン酸、リノ
ール酸、リルン酸、ステアロール酸等の炭素数10〜2
6個の脂肪酸(R。Dispersants used in the present invention include caprylic acid, capric acid, lauric acid, myristic acid, palmitic acid, stearic acid, behenic acid, oleic acid, elaidic acid, linoleic acid, lylunic acid, stearolic acid, etc. 10-2
6 fatty acids (R.
C0OH,R,は炭素数9〜25個のアルキル基)、前
記の脂肪酸のアルカリ金属(Li、Na、K等)または
アルカリ土類金属(Mg、Ca、Ba等)、NH,Φ
Cu、Pb等から成る金属石鹸、上記脂肪酸の脂肪酸ア
ミド;レシチン等が使用される。この他に炭素数4以上
の高級アルコール(ブタノール、オクチルアルコール、
ミリスチルアルコール、ステアリルアルコール)及びこ
れらのflA Mエステル、燐酸エステル、アミン化合
物等も使用可能である。また、ポリアルキレンオキサイ
ド及びこれらの硫酸エステル、燐酸エステル、アミン化
合物等やスルホ琥珀酸、スルホ琥珀酸エステル等も使用
可能である。これらの化合物にはバインダーとの相溶性
や特性を変えることからSi、Fの置換基を導入するこ
とも可能である。これらの分散剤は通常一種類以上で用
いられ、一種類の分散剤は結合剤100重量部に対して
0.005〜20重量部の範囲で添加される。これら分
散剤の使用方法は、強磁性粉末や非磁性粉末の表面に予
め被着させても良く、また分散途中で添加してもよい。COOH, R, is an alkyl group having 9 to 25 carbon atoms), alkali metals (Li, Na, K, etc.) or alkaline earth metals (Mg, Ca, Ba, etc.) of the above fatty acids, NH, Φ
Metal soaps made of Cu, Pb, etc., fatty acid amides of the above-mentioned fatty acids, lecithin, etc. are used. In addition, higher alcohols with 4 or more carbon atoms (butanol, octyl alcohol,
Myristyl alcohol, stearyl alcohol) and their flA M esters, phosphoric acid esters, amine compounds, etc. can also be used. Further, polyalkylene oxides and their sulfuric acid esters, phosphoric acid esters, amine compounds, etc., sulfosuccinic acid, sulfosuccinic acid esters, etc. can also be used. It is also possible to introduce Si and F substituents into these compounds in order to change their compatibility with the binder and their properties. One or more types of these dispersants are usually used, and one type of dispersant is added in an amount of 0.005 to 20 parts by weight per 100 parts by weight of the binder. These dispersants may be used by depositing them on the surface of the ferromagnetic powder or nonmagnetic powder in advance, or by adding them during dispersion.
このようなものは、例えば特公昭3928369号、特
公昭44−]77945号特公昭4B−15001号、
米国特許3387993号、同3470021号等に於
いて示されている。Such items include, for example, Special Publication No. 3928369, Special Publication No. 44-]77945, Special Publication No. 4B-15001,
This is shown in US Pat. No. 3,387,993, US Pat. No. 3,470,021, etc.
このほかに分散剤として好ましい化合物としては、カル
ボン酸、燐酸エステル等の界面活性剤やフ・ノ素系界面
活性剤フロラードFC95、FCl29、FC430,
FC431を用いる事ができる。In addition, preferred compounds as dispersants include surfactants such as carboxylic acids and phosphoric esters, and fluorochemical surfactants Florard FC95, FCl29, FC430,
FC431 can be used.
本発明の磁性層及び/またはバック層に使用される潤滑
剤、酸化防止剤としては、二硫化モリ7デン、窒化硼酸
、弗化黒鉛、炭酸カルシウム、硫酸バリウム、酸化硅素
、酸化チタン、酸化亜鉛、酸化錫、二硫化タングステン
等の無機微粉末、アクリルスチレン系樹脂微粉末、ヘン
ゾグアナミン系樹脂微粉末、メラミン系樹脂微粉末、ポ
リオレフィン系樹脂微粉末、ポリエステル系樹脂微粉末
、ポリアミド系樹脂微粉末、ポリイミド系樹脂微粉末、
ポリ弗化エチレン系樹脂微粉末等の樹脂微粉末、シリコ
ンオイル、脂肪酸変性シリコンオイル、グラファイト、
弗化アルコール、ポリオレフィン(ポリエチレンワック
ス等)、ポリグリコール(ポリエチレンオキシドワック
ス等)、テトラフルオロエチ1/ンオキソドワノクス、
ポリテトラフルオログリコール、パーフルオロ脂肪酸、
パーフルオロ脂肪酸エステル、パーフルオロアルキル硫
酸エステル、パーフルオロアルキル燐酸エステル、アル
キル塙酸エステル、ポリフェニルエーテル、炭素数10
〜40の一塩基性脂肪酸と炭素数3〜40個の一価のア
ルコールもしくは二価のアルコール、三価のアルコール
、四価のアルコール、六価のアルコールのいずれか1つ
もしくは2つ以上とから成る脂肪酸エステル類、炭素数
10個以上の一塩基性脂肪酸と該脂肪酸の炭素数と合計
して炭素数が11〜70個と成る一価〜六価のアルコー
ルから成る脂肪酸エステル類等の有機化合Th潤滑剤が
使用できる。又、炭素数8〜22の脂肪酸或いは脂肪酸
アミド、脂肪族アルコールも使用できる。これら有機化
合物潤滑剤の具体的な例としては、カプリル酸ブチル、
カプリル酸オクチル、ラウリン酸エチル、ラウリン酸ブ
チル、ラウリン酸オクチル、ミリスチン酸エチル、ミリ
スチン酸ブチル、ミリスチン酸エチル、バルミチン酸エ
チル、パルミチン酸ブチル、バルミチン酸オクナル、ス
テアリン酸エチル、ステアリン酸ブチル、ステアリン酸
オクチル、ステアリン酸アミル、モンクンワノクス、カ
ルナウハワソクス、バルミトン、10−−オキシバルミ
トン、綿ロウ、ミツロウ、羊毛ロウ、木ロウ、オシケラ
イト、石油ロウ、イー・ゲー・ロウ、アンヒドロソルビ
タンモノステアレート、アンヒドロソルビタンジステア
レート、アンヒドロソルビタン1−リステアレート、ア
ンヒドロソルビクンテトラステアレート、アンヒトロソ
ルビクンエチレンオキシドモノステアレート、オレイル
オレート、オレイルアルコール、ラウリルアルコール等
が有り単独若しくは組合わせ使用出来る。また本発明に
使用される潤滑剤としては所謂潤滑油添加剤も単独若し
くは組合わせで使用出来、酸化防止剤(アルキルフェノ
ール等)、錆どめ剤(ナフテン酸、アルケニルコハク酸
、ジラウリルフォスフェート等)、油性剤(ナタネ油、
ラウIJルアルコール等)、極圧剤(ジベンジルスルフ
ィド、トリクレジルフォスフェート、トリブチルホスフ
ァイト等)、清浄分散剤、粘度指数向上剤、流動点鋒下
剤、泡どめ剤等がある。これらの潤滑剤は結合剤100
重量部に対して0.05〜20重量部の範囲で添加され
る。Examples of lubricants and antioxidants used in the magnetic layer and/or back layer of the present invention include moly7denum disulfide, boric nitride, graphite fluoride, calcium carbonate, barium sulfate, silicon oxide, titanium oxide, and zinc oxide. , inorganic fine powder such as tin oxide, tungsten disulfide, acrylic styrene resin fine powder, Henzoguanamine resin fine powder, melamine resin fine powder, polyolefin resin fine powder, polyester resin fine powder, polyamide resin fine powder , polyimide resin fine powder,
Resin fine powder such as polyfluoroethylene resin fine powder, silicone oil, fatty acid modified silicone oil, graphite,
Fluorinated alcohol, polyolefin (polyethylene wax, etc.), polyglycol (polyethylene oxide wax, etc.), tetrafluoroethyl 1/n oxodowanox,
polytetrafluoroglycol, perfluoro fatty acid,
Perfluoro fatty acid ester, perfluoroalkyl sulfate, perfluoroalkyl phosphate, alkyl sulfate, polyphenyl ether, carbon number 10
~40 monobasic fatty acids and one or more of monohydric alcohol, dihydric alcohol, trihydric alcohol, tetrahydric alcohol, hexahydric alcohol having 3 to 40 carbon atoms Organic compounds such as fatty acid esters consisting of a monobasic fatty acid having 10 or more carbon atoms and a monohydric to hexavalent alcohol having a total carbon number of 11 to 70 carbon atoms. Th lubricant can be used. Furthermore, fatty acids or fatty acid amides and aliphatic alcohols having 8 to 22 carbon atoms can also be used. Specific examples of these organic compound lubricants include butyl caprylate,
Octyl caprylate, ethyl laurate, butyl laurate, octyl laurate, ethyl myristate, butyl myristate, ethyl myristate, ethyl valmitate, butyl palmitate, ocnal valmitate, ethyl stearate, butyl stearate, stearic acid Octyl, amyl stearate, Monkunwanox, Karnauhawasox, balmitone, 10-oxybalmitone, cotton wax, beeswax, wool wax, wood wax, oshikerite, petroleum wax, E.G. wax, anhydrosorbitan monostearate , anhydrosorbitan distearate, anhydrosorbitan 1-listearate, anhydrosorbitan tetrastearate, anhytrosorbicun ethylene oxide monostearate, oleyl oleate, oleyl alcohol, lauryl alcohol, etc., which can be used alone or in combination. . In addition, so-called lubricating oil additives can be used alone or in combination as the lubricant used in the present invention, such as antioxidants (alkylphenols, etc.), rust inhibitors (naphthenic acid, alkenylsuccinic acid, dilauryl phosphate, etc.). ), oily agents (rapeseed oil,
(eg, alcohol), extreme pressure agents (dibenzyl sulfide, tricresyl phosphate, tributyl phosphite, etc.), detergent dispersants, viscosity index improvers, pour point laxatives, anti-foaming agents, etc. These lubricants are binder 100
It is added in an amount of 0.05 to 20 parts by weight.
また、酸化防止剤としてはベンゾトリアジン、ベンゾチ
アゾール、ベンゾジアジン、EDTA等の複素環化合物
、複素化合物を用いる事ができる。Further, as the antioxidant, heterocyclic compounds and heterocompounds such as benzotriazine, benzothiazole, benzodiazine, and EDTA can be used.
本発明に用いる帯電防止剤としてはグラファイト、カー
ボンブラック、カーボンブラックグラフトポリマー、酸
化錫−酸化アンチモン、酸化錫、酸化チタン−酸化錫−
酸化アンチモン、等の導電性粉末;サポニン等の天然界
面活性剤;アルキレンオキサイド系、グリセリン系、グ
リシドール系、多価アルコール、多価アルコールエステ
ル、アルキルフェノールE○付加体等のノニオン界面活
性剤;高級アルキルアミン類、環状アミン、ヒダントイ
ン誘導体、アミドアミン、エステルアミド、第四級アン
モニウム塩類、ピリジンそのほかの複素環類、ホスホニ
ウムまたはスルホニウム類、等のカチオン界面活性剤;
カルボン酸、スルホン酸、燐酸、硫酸エステル基、燐酸
エステル基などの酸性基を含むアニオン界面活性剤;ア
ミノ酸類;アミノスルホン酸類、アミノアルコールの硫
酸または燐酸エステル類、アルキルベタイン型等の両性
界面活性剤等が使用される。これらの界面活性剤は単独
または混合して添加しても良い。また、これらの界面活
性剤は磁気記録媒体の表面にImg/ボ〜550 m
g / rrfオーバーコートしても良い。The antistatic agents used in the present invention include graphite, carbon black, carbon black graft polymer, tin oxide-antimony oxide, tin oxide, titanium oxide-tin oxide-
Conductive powders such as antimony oxide; natural surfactants such as saponin; nonionic surfactants such as alkylene oxides, glycerin, glycidol, polyhydric alcohols, polyhydric alcohol esters, and alkylphenol E○ adducts; higher alkyl Cationic surfactants such as amines, cyclic amines, hydantoin derivatives, amidoamines, ester amides, quaternary ammonium salts, pyridine and other heterocycles, phosphoniums or sulfoniums;
Anionic surfactants containing acidic groups such as carboxylic acid, sulfonic acid, phosphoric acid, sulfuric ester groups, and phosphoric ester groups; Amino acids; Ampholytic surfactants such as amino sulfonic acids, sulfuric acid or phosphoric acid esters of amino alcohols, and alkyl betaine types. agents etc. are used. These surfactants may be added alone or in combination. Moreover, these surfactants can be applied to the surface of the magnetic recording medium at a concentration of Img/bo~550 m
g/rrf overcoat may be used.
磁気記録媒体における、これらの界面活性剤の使用量は
、強磁性粉末100重量部当たり0.01〜10重量部
である。これらは帯電防止剤として用いられるものであ
るが、時としてそのほかの目的、例えば分散、磁気特性
の改良、潤滑性の改良、塗布助剤として適用される場合
もある。The amount of these surfactants used in the magnetic recording medium is 0.01 to 10 parts by weight per 100 parts by weight of the ferromagnetic powder. Although these are used as antistatic agents, they are sometimes used for other purposes, such as dispersion, improving magnetic properties, improving lubricity, and as coating aids.
本発明に使用されるカーボンブラックとしてはゴム用フ
ァーネス、ゴム用サーマル、カラー用ブラ、り等を挙げ
ることができる。Examples of the carbon black used in the present invention include rubber furnaces, rubber thermals, color bras, and the like.
カーボンブラックの米国における略称の具体例をしめす
と、SAF 、l5AF、 T]SAF 、 T 、
)IAF 、 SPF X FF、 FEF 、
、 HMF 、、 GPF 、 八PF 、、
5FIF 、 門PF 2ECF 、 CF、、F
T、 MT 、HCC、M針、LFF 、、RCF等
があり、米国のASTM規格のD−1765−82aに
分類されているものを使用することができる。本発明に
使用されるこれらカーボンブランクの平均粒子サイズは
5〜101000n電子顕微鏡)、窒素吸着法比表面積
は1〜1500ボ/g、 pHは2〜13(JIS規格
に一62211982法)、ジブチルフタレート(DB
P)給油量は5〜2000m1/100g(JIS規格
に−6221−1982法)である。本発明に使用され
るカーボンブランクの含水率は0.00〜20−tχで
ある。本発明に使用されるカーボンブラックのサイズは
、塗布膜の表面電気抵抗を下げる目的で5〜1100n
のカーボンブランクを、また塗布膜の強度を制御すると
きに50〜1000nIIlのカーボンブラックを使用
することができる。Examples of abbreviations for carbon black in the United States include SAF, l5AF, T]SAF, T,
) IAF, SPF X FF, FEF,
, HMF , , GPF , 8PF , ,
5FIF, Gate PF 2ECF, CF,,F
There are T, MT, HCC, M needles, LFF, RCF, etc., and those classified as D-1765-82a of the American ASTM standard can be used. The average particle size of these carbon blanks used in the present invention is 5 to 101,000 nm (electron microscope), the specific surface area by nitrogen adsorption method is 1 to 1,500 bo/g, the pH is 2 to 13 (JIS standard-62211982 method), and dibutyl phthalate. (DB
P) The amount of oil supplied is 5 to 2000 m1/100 g (JIS standard -6221-1982 method). The moisture content of the carbon blank used in the present invention is 0.00 to 20-tχ. The size of the carbon black used in the present invention is 5 to 1100 nm for the purpose of lowering the surface electrical resistance of the coating film.
carbon blank and 50 to 1000 nIIl of carbon black can be used when controlling the strength of the coating film.
また塗布膜の表面粗さを制御する目的でスペーシングロ
ス減少のための平滑化のためにより微粒子のカーボンブ
ラック(loOnm以下)を、粗面化して摩擦係数を下
げる目的で粗粒子のカーボンブランク(50nm以上)
用いることができる。このようにカーボンブランクの種
類と添加量は磁気記録媒体に要求される目的に応じて使
い分こすられる。In addition, in order to control the surface roughness of the coating film, finer particle carbon black (loOnm or less) was used for smoothing to reduce spacing loss, and coarser particle carbon blank (lower than loOnm) was used to roughen the surface and lower the coefficient of friction. 50nm or more)
Can be used. In this way, the type and amount of carbon blank to be added are determined depending on the purpose required for the magnetic recording medium.
また、これらのカーホンブラ、りを、後述の分散剤など
で表面処理したり、樹脂でグラフト化して使用してもよ
い。また、カーボンブランクを製造するときの炉の温度
を2000°C以上で処理して表面の一部をグラファイ
ト化したものも使用できる。Furthermore, these carphone bras may be surface-treated with a dispersant described below or grafted with a resin before use. Further, a carbon blank whose surface is partially graphitized by processing the furnace at a temperature of 2000° C. or higher when manufacturing the carbon blank can also be used.
また、特殊なカーボンブラックとして中空カーボンブラ
ンクを使用することもできる。Moreover, a hollow carbon blank can also be used as a special carbon black.
これらのカーボンブラ、りは磁性層の場合、強磁性粉末
100重量部に対して0.1〜20重量部で用いること
が望ましく、また、ハ、り層の場合は、バック層真上に
存在する同一塗布面積の強磁性粉未重量に対し、好まし
くは0. 1〜100χの範囲、バック層バインダー重
量に対し30〜300χの範囲が望ましい。In the case of a magnetic layer, it is desirable to use 0.1 to 20 parts by weight of these carbon bras per 100 parts by weight of ferromagnetic powder. Preferably, the weight of the ferromagnetic powder is 0. It is preferably in the range of 1 to 100 χ, and preferably in the range of 30 to 300 χ based on the weight of the back layer binder.
本発明に使用できるカーボンブランクは、例えば、「カ
ーボンブラック便覧J、カーボンブラック協会編(昭和
46年発行)を参考にすることができる。For carbon blanks that can be used in the present invention, for example, "Carbon Black Handbook J," edited by the Carbon Black Association (published in 1972) can be referred to.
本発明においては、バック層及び/または磁性層には研
磨剤を使用することができる。本発明に用いる研磨剤と
しては一般に使用される研磨作用若しくは琢磨作用をも
つ材料で、熔融アルミナ、α−アルミナ、T−アルミナ
、α−γ−アルミナ、炭化硅素、酸化クロム、酸化セリ
ウム、コランダム、人造ダイヤモンド、α−酸化鉄、ザ
クロ石、ユメリーC主成分:コランダムと磁鉄鉱)、ガ
ーネット、珪石、窒化硅素、窒化硼素、炭化モリブデン
、炭化硼素、炭化タングステン、チタンカーバイド、ク
ォーツ、トリポリ、珪藻土、ドロマイト等で、主として
モース硬度6以上より好ましくはモース硬度8以上の材
料が1内示4種迄の組合わせで使用される、これらの研
磨剤は平均粒子サイズが0.005〜5ミクロンの大き
さのものが使用され、特に好ましくは0.01〜2ミク
ロンである。また、本発明では、これら研磨剤の含水率
を0.00〜1.00重景%の範囲まで拡張した品位の
ものを使用できる。これらの研磨剤は結合剤100重量
部に対して0.01〜20M量部の範囲で添加される。In the present invention, an abrasive can be used for the back layer and/or the magnetic layer. The abrasive used in the present invention is a commonly used material with an abrasive or polishing action, such as fused alumina, α-alumina, T-alumina, α-γ-alumina, silicon carbide, chromium oxide, cerium oxide, corundum, Artificial diamond, α-iron oxide, garnet, Yumery C (main components: corundum and magnetite), garnet, silica, silicon nitride, boron nitride, molybdenum carbide, boron carbide, tungsten carbide, titanium carbide, quartz, tripoli, diatomaceous earth, dolomite etc., materials with a Mohs hardness of 6 or more, preferably 8 or more, are used in combinations of up to 4 types in 1. These abrasives have an average particle size of 0.005 to 5 microns. 0.01 to 2 microns is particularly preferred. In addition, in the present invention, these abrasives whose water content is expanded to a range of 0.00 to 1.00% can be used. These abrasives are added in an amount of 0.01 to 20 M parts per 100 parts by weight of the binder.
これらの研磨剤は磁性層の場合、強磁性粉末100重量
部に対して1〜15重量部で用いることが望ましく、ま
た、バック層の場合は、ハ・ツク層真上に存在する同一
塗布面積の強磁性粉末重量に対し0.001〜10.O
Xの範囲、バック層バインダー重量に対し0.1〜10
.OXの範囲が望ましい。In the case of a magnetic layer, these abrasives are preferably used in an amount of 1 to 15 parts by weight per 100 parts by weight of ferromagnetic powder, and in the case of a back layer, they are used in the same coating area directly above the hard layer. of ferromagnetic powder weight from 0.001 to 10. O
Range of X, 0.1 to 10 based on back layer binder weight
.. A range of OX is desirable.
本発明の分散、混練、塗布の際に使用する有機溶媒とし
ては、任意の比率でアセトン、メチルエチルケトン、メ
チルイソブチルケトン、シクロヘキサノン、イソホロン
、テトラヒドロフラン等のケトン系;メタノール、エタ
ノール、プロパツール、ブタノール、イソブチルアルコ
ール、イソプロピルアルコール、メチルシクロヘキサノ
ールなどのアルコール系;酢酸メチル、酢酸エチル、酢
酸ブチル、酢酸イソブチル、酢酸イソプロピル、乳Mエ
チル、酢酸グリコールモノエチルエーテル等のエステル
系;ジエチルエーテル、テトラヒドロフラン、グリコー
ルジメチルエーテル、グリコールモノエチルエーテル、
ジオキサンなどのエーテル系;ヘンゼン、トルエン、キ
シレン、フレソール、クロルヘンゼン、スチレンなどの
タール系(芳香族炭化水素);メチレンクロライド、エ
チレンクロライド、四塩化炭素、クロロホルム、エチレ
ンクロルヒドリン、ジクロルベンゼン等の塩素化炭化水
素、N、N−ジメチルホルムアルデヒド、ヘキサン等の
ものが使用できる。Organic solvents used in the dispersion, kneading, and coating of the present invention include ketones such as acetone, methyl ethyl ketone, methyl isobutyl ketone, cyclohexanone, isophorone, and tetrahydrofuran; methanol, ethanol, propatool, butanol, and isobutyl; Alcohols such as alcohol, isopropyl alcohol, methylcyclohexanol; esters such as methyl acetate, ethyl acetate, butyl acetate, isobutyl acetate, isopropyl acetate, milk ethyl acetate, glycol monoethyl acetate; diethyl ether, tetrahydrofuran, glycol dimethyl ether, glycol monoethyl ether,
Ethers such as dioxane; tars (aromatic hydrocarbons) such as henzene, toluene, xylene, Fresol, chlorhenzene, and styrene; methylene chloride, ethylene chloride, carbon tetrachloride, chloroform, ethylene chlorohydrin, dichlorobenzene, etc. Chlorinated hydrocarbons, N,N-dimethylformaldehyde, hexane and the like can be used.
分散、混線の方法には特に制限はなく、また各成分の添
加順序などは上記本発明に反しない範囲で適宜設定する
ことができる。磁性塗料およびバック層塗料の調製には
通常の混練機、例えば、二本ロールミル、三本ロールミ
ル、ボールミル、ペブルミル、トロンミル、サンドグラ
インダー、ゼグパリ(Szegvari)、アトライタ
ー、高速インペラー、分散機、高速ストーンミル、高速
度衝撃ミル、デイスパー、ニーグー、高速ミキサリボン
ブレンダー、コニーダー、インテンシブミキサー、タン
ブラ−、ブレンダー、ディスパーザ−、ホモジナイザー
、単軸スクリュー押し出し機、二輪スクリュー押し出し
機、及び超音波分散機などを用いることができる。混線
分散に関する技術の詳細は、T、C,PATTON著(
チーシー、パントン) ” Pa1nt Flow
and Pigment旧5persion (ペイ
ント フロー アンド ピグメント ディスバージョン
)1964年John Wiley& 5ons社発行
(ジョン ウィリー アント サンプ)や田中信−著「
工業材料」25巻37(1977)などや当該書籍の引
用文献に記載されており、連続処理の為これらの混線分
散機を適宜組み合わせ混練、分散、混合、送液し塗布す
る。また、米国特許第2581414号及び同第285
5156号などの明細書にも記載がある。本発明におい
ても上記の書籍や当該書籍の引用文献などに記載された
方法に準じて混線分散を行い磁性塗料およびバック層塗
料を調製することができる。There are no particular restrictions on the method of dispersion and cross-talk, and the order of addition of each component can be appropriately set within the scope of the present invention. For the preparation of magnetic paints and back layer paints, conventional kneading machines are used, such as two-roll mills, three-roll mills, ball mills, pebble mills, thoron mills, sand grinders, Szegvari, attritors, high-speed impellers, dispersers, high-speed stones. Using mills, high-speed impact mills, dispers, negoos, high-speed mixers, ribbon blenders, co-kneaders, intensive mixers, tumblers, blenders, dispersers, homogenizers, single-screw extruders, two-wheel screw extruders, ultrasonic dispersers, etc. be able to. For details on the technology related to crosstalk dispersion, please refer to the book written by T. C. PATTON (
Cheesy, Pantone) ” Pa1nt Flow
and Pigment former 5persion (Paint Flow and Pigment Disversion) published by John Wiley & 5ons in 1964 (John Wiley Ant Thump) and Shin Tanaka.
"Industrial Materials" vol. 25, 37 (1977), and the cited literature of the book, and for continuous processing, these intermixing dispersion machines are appropriately combined to knead, disperse, mix, feed and apply. Also, U.S. Patent No. 2581414 and U.S. Patent No. 285
It is also described in specifications such as No. 5156. In the present invention, the magnetic paint and the back layer paint can also be prepared by carrying out crosstalk dispersion according to the method described in the above-mentioned book or the cited literature of the book.
磁性層の形成は上記の組成などを本発明に反しない範囲
で任意に組合せて有機溶媒に溶解し、本発明に使用する
磁性層塗布液を調製して支持体上に塗布・乾燥する。テ
ープとして使用する場合には支持体の厚み2.5〜10
0ミクロン程度、好ましくは3〜70ミクロン程度が良
い。ディスクもしくはカード状の場合は厚みが0.03
〜10順程度であり、ドラムの場合は円筒状で用いる事
も出来る。素材としてはポリエチレンテレフタレート、
ポリエチレンナフタレート等のポリエステル類、ポリプ
ロピレン、ポリエチレン等ポリオレフィン類、セルロー
ストリアセテート、セルロースダイアセテート等のセル
ロース誘導体、ポリ塩化ビニル、ポリ塩化ビニリデン等
のビニル系樹脂類、ポリカーボネート、ポリアミド、ポ
リスルホン等のプラスチックのほかにアルミニウム、銅
等の金属、ガラス等のセラミックス等も使用出来る。こ
れらの支持体は塗布に先立って、コロナ放電処理、プラ
ズマ処理、下塗処理、熱処理、除塵埃処理、金属蒸着処
理、アルカリ処理をおこなってもよい。The magnetic layer is formed by arbitrarily combining the above-mentioned compositions within a range not contrary to the present invention and dissolving them in an organic solvent to prepare a magnetic layer coating solution for use in the present invention, which is then coated onto a support and dried. When used as a tape, the thickness of the support is 2.5 to 10
The thickness is about 0 microns, preferably about 3 to 70 microns. If it is in the form of a disk or card, the thickness is 0.03
~10 order, and in the case of a drum, it can also be used in a cylindrical shape. The material is polyethylene terephthalate,
Polyesters such as polyethylene naphthalate, polyolefins such as polypropylene and polyethylene, cellulose derivatives such as cellulose triacetate and cellulose diacetate, vinyl resins such as polyvinyl chloride and polyvinylidene chloride, and plastics such as polycarbonate, polyamide, and polysulfone. Metals such as aluminum and copper, and ceramics such as glass can also be used. Prior to coating, these supports may be subjected to corona discharge treatment, plasma treatment, undercoating treatment, heat treatment, dust removal treatment, metal vapor deposition treatment, and alkali treatment.
これら支持体に関しては例えば***特許3338854
A、特開昭59−116926号、米国特許43883
68号;三石幸夫著、 「繊維と工業」31巻 p5
0〜55.1975年などに記載されている。Regarding these supports, for example, West German Patent No. 3338854
A, JP 59-116926, U.S. Patent No. 43883
No. 68; Yukio Mitsuishi, “Textiles and Industry” Volume 31, p5
0 to 55. Described in 1975, etc.
支持体上へ前記の磁性層及び/またはバック層を塗布す
る方法としてはエアードクターコート、ブレードコート
、エアナイフコート、スクイズコート、含浸コート、リ
バースロールコート、トランスファーロールコ−1・、
グラビアコート、キスコート、キャストコート、スプレ
ィコート、バーコード、スピンコード等が利用出来、そ
の他の方法も可能であり、これらの具体的説明は浅倉書
店発行の「コーティング工業」253頁〜277頁(昭
和46.3.20.発行)に詳細に記載されている。Methods for coating the magnetic layer and/or back layer on the support include air doctor coating, blade coating, air knife coating, squeeze coating, impregnation coating, reverse roll coating, transfer roll coating,
Gravure coat, kiss coat, cast coat, spray coat, bar code, spin code, etc. can be used, and other methods are also possible. Specific explanations of these methods can be found in "Coating Industry" published by Asakura Shoten, pages 253 to 277 (Showa 46.3.20. Issue).
このような方法により、支持体上に塗布された磁性層は
必要により層中の強磁性粉末を直ちに乾燥しながら所望
の方向へ配向させる処理を施したのち、形成した磁性層
を乾燥する。このときの支持体の搬送速度は、通常10
m/分〜1000m/分でおこなわれ、乾燥温度が20
°C〜130°Cで制御される。又必要により表面平滑
化加工を施したり、所望の形状に裁断したりして、本発
明の磁気記録体を製造する。これらの製造方法はフィラ
ーの表面処理、混練・分散、塗布、熱処理、カレンダー
放射線照射(EB)処理、表面研磨処理、裁断の工程を
連続して行う事が好ましい。また必要に応して幾つかに
工程を分りる事ができる。By such a method, the magnetic layer coated on the support is immediately subjected to a treatment to orient the ferromagnetic powder in the layer in a desired direction while drying, if necessary, and then the formed magnetic layer is dried. The transport speed of the support at this time is usually 10
m/min to 1000 m/min, and the drying temperature is 20 m/min to 1000 m/min.
Controlled between °C and 130°C. Further, the magnetic recording body of the present invention is manufactured by subjecting it to surface smoothing processing and cutting it into a desired shape, if necessary. In these manufacturing methods, it is preferable that the steps of surface treatment of the filler, kneading/dispersion, coating, heat treatment, calendar radiation irradiation (EB) treatment, surface polishing treatment, and cutting are performed continuously. You can also divide the process into several parts if necessary.
これらの工程においては、温度、湿変が制j卸され、温
度は10°C−130’、イ・容度は空気中の水分量で
表すと、5 m g / rrf〜20 m g /
rrrである。In these processes, temperature and humidity changes are controlled, and the temperature is 10°C-130', and the capacity is 5 mg/rrf to 20 mg/rrf, expressed as the amount of moisture in the air.
It is rrr.
これらは、例えば、特公昭40−23625号公報、特
公昭39−28368号公報、末日特許第347396
0号明細書、等にしめされている。These include, for example, Japanese Patent Publication No. 40-23625, Japanese Patent Publication No. 39-28368, and Latter-day Patent No. 347396.
It is shown in the specification of No. 0, etc.
又、特公昭41−131.81号公報にしめされる方法
はこの分野における基本的、且つ重要な技f4iと考え
られている。Furthermore, the method disclosed in Japanese Patent Publication No. 41-131.81 is considered to be a basic and important technique f4i in this field.
又、本発明は、磁性層、バック層が多層構造の場合も包
含され、この場合、各層の塗布液は、本発明に従って各
々調製されるが、塗布法としては各塗布液を湿潤状態重
畳して塗布するいわゆるウエノトオンウエント塗布方式
が好ましい。The present invention also includes cases where the magnetic layer and the back layer have a multilayer structure. In this case, the coating liquid for each layer is prepared according to the present invention, and the coating method is to superimpose each coating liquid in a wet state. A so-called wet-on-wet coating method is preferred.
ウェットオンウェット方式としては特開昭611399
29号公報に記載の塗布方法を用いることができる。As a wet-on-wet method, Japanese Patent Application Laid-Open No. 611399
The coating method described in Japanese Patent No. 29 can be used.
(発明の効果]
本発明は、カルボジイミド基含有化合物である本発明の
化合物を使用することにより、塗布液中に存在する水を
カルボジイミド基と反応させることにより除去し、磁性
層及びもしくはバック層のバインダーのポリイソイアネ
ート化合物のイソシアネート基の水との反応を極力防止
することにより、従来生成されていたイソシアネ−H5
,1120、およびイソシアネーt4からなる結合反応
を低減させると共にイソシアネート基の当量数を確保し
て、バインダーの官能基と充分に反応してl19の硬化
反応が効率よく進行せしめて三次元網目構造を従来より
密に形成することができるので、ヤング率が改善され、
かつ耐久性を著しく向上せしめた磁気記録媒体が得られ
る。(Effects of the Invention) The present invention uses the compound of the present invention, which is a carbodiimide group-containing compound, to remove water present in the coating solution by reacting with the carbodiimide group, thereby removing water from the magnetic layer and/or back layer. By preventing the reaction of the isocyanate group of the polyisocyanate compound of the binder with water as much as possible, the isocyane-H5 that was conventionally produced
, 1120, and isocyanate t4, as well as ensuring the equivalent number of isocyanate groups, sufficiently reacting with the functional groups of the binder, and allowing the curing reaction of 119 to proceed efficiently, resulting in a three-dimensional network structure similar to that of the conventional one. Since it can be formed more densely, Young's modulus is improved,
In addition, a magnetic recording medium with significantly improved durability can be obtained.
また、本発明の磁気記録媒体は、磁性N塗布液の調製に
おいて強磁性粉末、カーボンブラック、研磨剤等の無機
粉体を種類別に別個に溶剤に分散することにより、無機
粉体の分散性が向上すると共に効果的な水分除去が行わ
れるため磁性層の膜強化と共に表面性をも改善し高S/
Nを得ることができる。In addition, in the magnetic recording medium of the present invention, the dispersibility of the inorganic powder is improved by separately dispersing inorganic powder such as ferromagnetic powder, carbon black, and abrasive in a solvent according to the type in preparing the magnetic N coating liquid. At the same time, effective water removal is carried out, which strengthens the magnetic layer and improves surface properties, resulting in high S/
It is possible to obtain N.
[実施例〕
以下に本発明を実施例により更に具体的に説明する。こ
こに示す成分、割合、操作順序等は本発明の精神から逸
脱しない範囲において変更しうるものであることは本業
界に携わるものにとっては容易に理解されることである
。[Example] The present invention will be explained in more detail below with reference to Examples. It will be readily understood by those skilled in the art that the ingredients, proportions, order of operations, etc. shown herein may be modified without departing from the spirit of the invention.
従って、本発明は下記の実施例に制限されるべきではな
い。尚、実施例及び比較例中の部は重量部をしめす。Therefore, the invention should not be limited to the examples below. In addition, parts in Examples and Comparative Examples indicate parts by weight.
(実施例1〕
下記磁性層塗布液を磁性層塗布液用組成液〔IIをニー
ダ−に入れ充分混練した後、別分散同組成液(It)及
び(III)を追加投入し、充分混練し、塗布前に本発
明の化合物(■〕、続いてポリイソイアネート化合物含
有組成液[X′]を入れ混合分散して作成した。(Example 1) The following magnetic layer coating solution was added to a magnetic layer coating solution composition [II] in a kneader and thoroughly kneaded, then separately dispersed same composition solutions (It) and (III) were added and thoroughly kneaded. The compound of the present invention (■) was then mixed and dispersed with the polyisocyanate compound-containing composition solution [X'] before coating.
磁性層塗布液
[1) Co含有1−FezO,、粉末 30
0部(窒素吸着比表面積35rn / g、 Fe”=
3aLom!、粉末)1c=9000e )
塩化ビニル酢酸ビニル樹脂 30部(400X l
l0A、日本ゼオン社製)ポリウレタン樹脂
10部オレイン酸 1部シク
ロへキサノン 150部(II)カーボン
ブランク 12部(コンダクテノクスSC
、コロンビアン社製、平均粒子サイズ20rv)
塩化ビニル酢酸ビニル樹脂 5部
ポリウレタン樹脂 3部
メチルエチルケトン 100部(111)研磨
剤:α−アルミナ 18部(住人化学社製、旧
T50)
塩化ビニル酢酸ビニル樹脂 5部
ポリウレタン樹脂 3部
メチルエチルケトン 100部[TV〕本発明
の化合物 X部(ジシクロへキンルカル
ボシイミ)・)〔v]ポリイソイアネート化合物
24部(コロネート3040、バイエル社製)ステアリ
ン酸 3部イソ]・リゾシルステア
レート 6部酢酸ブチル 10
0部この磁性層塗布液を粘度調整した後、厚さ15−の
ポリエチレンテレフタレート上に乾燥膜厚が、5.0岬
で塗布し、その侭3000ガウスの磁石で磁場配向した
後乾燥し、引き続きカレンダーをかけて磁性層を作成し
た。引き続き磁性層を設けた非磁性支持体の裏側に、下
記パック層塗布液用組成液[IIをボールミルで混線分
散し、本発明の化合物[I[)続いて同組成液(III
)を加えて混合撹拌してパック層塗布液を調整し、乾燥
厚み1.0−に塗布してバック層を設けた。Magnetic layer coating liquid [1] Co-containing 1-FezO, powder 30
0 parts (Nitrogen adsorption specific surface area 35rn/g, Fe”=
3aLom! , powder) 1c=9000e) Vinyl chloride vinyl acetate resin 30 parts (400X l
l0A, Nippon Zeon Co., Ltd.) polyurethane resin
10 parts Oleic acid 1 part Cyclohexanone 150 parts (II) Carbon blank 12 parts (Conductenox SC
(Manufactured by Columbian, average particle size 20rv) Vinyl chloride vinyl acetate resin 5 parts Polyurethane resin 3 parts Methyl ethyl ketone 100 parts (111) Abrasive: α-Alumina 18 parts (Manufactured by Sumima Kagaku, former T50) Vinyl chloride vinyl acetate resin 5 parts polyurethane resin 3 parts methyl ethyl ketone 100 parts [TV] Compound of the present invention
24 parts (Coronate 3040, manufactured by Bayer AG) Stearic acid 3 parts Iso]-lysosyl stearate 6 parts Butyl acetate 10
0 parts After adjusting the viscosity of this magnetic layer coating solution, it was coated on polyethylene terephthalate with a thickness of 15 mm to a dry film thickness of 5.0 cape, and after being oriented in a magnetic field using a magnet with a pitch of 3000 Gauss, it was dried, and then A magnetic layer was created by calendering. Subsequently, on the back side of the non-magnetic support provided with the magnetic layer, the following pack layer coating solution composition [II] was mixed and dispersed in a ball mill, and the compound of the present invention [I[] was then mixed with the same composition solution (III).
) was mixed and stirred to prepare a pack layer coating solution, which was coated to a dry thickness of 1.0 - to provide a back layer.
パック層塗布液
cl)カーボンブランク 20部(レーベ
ンMTP 、窒素吸着比表面積:10ホ/g、平均粒子
サイズ250 nm、キャボ7)社製)
カーボンブラ、り 8o部(ハルカン×0
72、窒素吸着比表面積:160nf/g、平均粒子サ
イズ30 nm、キャボソト社製)
ポリウレタンポリカーボネーI−樹脂
(FJ2、大日精化社製) 60部フェノ
キシ樹脂 20部
メチルエチルケトン 700部シクロへキサ
ノン 3oo部(It)本発明の化合物
Y部(ジシクロへキシルカルボジイミ
ド)
EV)ポリイソイアネート化合物 15部(コロネ
ート3040.日本ポリウレタン社製)潤滑剤
0.1部(シリコーン:信越化学社製
)
潤滑剤 1 部(オレイン酸
)
メチルエチルケトン 100部この後、】7
2インチ幅にスリットして、ビデオ・テープを作成だ。Pack layer coating liquid cl) Carbon blank 20 parts (Leben MTP, nitrogen adsorption specific surface area: 10/g, average particle size 250 nm, manufactured by Cabo7) Carbon blank 8 parts (Harkan x 0)
72, Nitrogen adsorption specific surface area: 160 nf/g, average particle size 30 nm, manufactured by Cabosoto Co., Ltd.) Polyurethane polycarbonate I-resin (FJ2, manufactured by Dainichiseika Co., Ltd.) 60 parts Phenoxy resin 20 parts Methyl ethyl ketone 700 parts Cyclohexanone 30 parts (It) Compound of the present invention
Part Y (dicyclohexylcarbodiimide) EV) Polyisocyanate compound 15 parts (Coronate 3040. Manufactured by Nippon Polyurethane Co., Ltd.) Lubricant
0.1 part (silicone: manufactured by Shin-Etsu Chemical Co., Ltd.) Lubricant 1 part (oleic acid) Methyl ethyl ketone 100 parts After this, ]7
Create a video tape by slitting it into 2-inch widths.
(実施例2〜5、比較例1〜4〕
実施例1において、ジシクロカルボジイミドの添加量X
部、Y部を表1のように変更してテープを作成し、他は
実施例1と同様にサンプルを作成した。(Examples 2 to 5, Comparative Examples 1 to 4) In Example 1, the amount of dicyclocarbodiimide added
A tape was prepared by changing the part and Y part as shown in Table 1, and a sample was prepared in the same manner as in Example 1 except for the other parts.
〔実施例6(参考例)〕
実施例1において、磁性層組成物の別分散〔m)、(I
II)を同一量、同一組成で(1)において同時分散を
行った。[Example 6 (Reference Example)] In Example 1, different dispersion of the magnetic layer composition [m), (I
II) was simultaneously dispersed in (1) using the same amount and the same composition.
得られた上記実施例1〜6、比較例1〜4のサンプルの
CS/N、走行耐久性を評価し、その結果も合わせて表
1に示した。The obtained samples of Examples 1 to 6 and Comparative Examples 1 to 4 were evaluated for CS/N and running durability, and the results are also shown in Table 1.
CS/N:室温(23°C150%RH)において、1
部2インチVTRでCS/Nを測定した。CS/N: 1 at room temperature (23°C 150%RH)
CS/N was measured using a 2-inch VTR.
走行耐久性(D、O,) :室温(23°C150%R
H)において、1部2インチVTRでドロップアウトを
測定(初期値)した後、繰り返し走行100バスし、ビ
デオ・テープを40°C180%RH(相対湿度)で1
週間保管後室温に戻し、再びドロップアウトを測定(経
時値)し、1分間あたりのドロップアウトの経時値とド
ロップアウトの初期値との差の個数を求めた。Running durability (D, O,): Room temperature (23°C 150% R
In H), after measuring the dropout (initial value) with a 2-inch VTR, it was repeatedly run 100 times, and the video tape was heated at 40°C and 180% RH (relative humidity).
After storage for a week, the sample was returned to room temperature, and the dropout was measured again (time-lapse value), and the difference in number of dropouts per minute between the time-lapse value and the initial dropout value was determined.
走行耐久性(静止画像)
室温(23℃、60%RH)において、1部2インチV
TRで走行荷重を2倍にして静止画像モードで再生し、
出力の一16dBとなるまでの時間を調べた。Running durability (still image) At room temperature (23°C, 60% RH), 1 part 2 inch V
Double the running load with TR and play in still image mode,
The time required for the output to reach -16 dB was investigated.
本発明の磁気記録媒体は、表1の実施例の結果から明ら
かのように、ドロップアウト、静止画像特性が優れた性
能を示している。比較例の場合は、塗布液中の水分が過
剰で、ポリイソイアネート化合物硬化剤の有効な架橋が
阻害されていると考えられ塗布膜のヤング率が非常に低
下しており磁気記録媒体として不適切であると認められ
る。また、実施例6(参考例)から別分散がS/Hの点
から有利であることが認められる。As is clear from the results of the examples shown in Table 1, the magnetic recording medium of the present invention exhibits excellent dropout and still image characteristics. In the case of the comparative example, the Young's modulus of the coating film was extremely low, probably due to excessive water content in the coating solution and inhibiting the effective crosslinking of the polyisocyanate compound curing agent, making it difficult to use as a magnetic recording medium. Approved to be inappropriate. Further, from Example 6 (reference example), it is recognized that separate dispersion is advantageous from the viewpoint of S/H.
手続補装置 平成3年 1月28日procedural aids 1991 January 28th
Claims (4)
を塗布して非磁性支持体上に磁性層を設けてなる磁気記
録媒体において、該磁性層塗布液は、カルボジイミド基
含有化合物が含有せしめられた後、ポリイソイアネート
化合物が含有せしめられてなるものであることを特徴と
する磁気記録媒体。(1) In a magnetic recording medium in which a magnetic layer is provided on a nonmagnetic support by coating a magnetic layer coating solution containing ferromagnetic powder and a binder, the magnetic layer coating solution contains a carbodiimide group-containing compound. 1. A magnetic recording medium characterized in that the magnetic recording medium is made to contain a polyisocyanate compound.
バインダーを含むバック層塗布液を塗布して設けられた
バック層を有し、該バック層塗布液は、カルボジイミド
基含有化合物が含有せしめられた後、ポリイソイアネー
ト化合物が含有せしめられてなるものであることを特徴
とする請求項1記載の磁気記録媒体。(2) A back layer is provided by coating a back layer coating liquid containing a binder on the opposite side of the nonmagnetic support surface on which the magnetic layer is provided, and the back layer coating liquid contains a carbodiimide group-containing compound. 2. The magnetic recording medium according to claim 1, wherein the magnetic recording medium is further impregnated with a polyisocyanate compound.
カルボジイミド基含有化合物を磁性層及び/またはバッ
ク層に含浸させてなることを特徴とする請求項1または
2記載の磁気記録媒体。(3) After coating and drying the magnetic layer and/or back layer,
3. The magnetic recording medium according to claim 1, wherein the magnetic layer and/or back layer is impregnated with a carbodiimide group-containing compound.
組成量からなる2種以上の該磁性層塗布液用組成物を混
合して調製された該磁性層塗布液を磁性層に塗布してな
ることを特徴とす請求項1〜3の何れか1項記載の磁気
記録媒体。(4) The magnetic layer is coated with the magnetic layer coating liquid prepared by mixing two or more magnetic layer coating liquid compositions having mutually different compositional components and/or mutually different composition amounts. The magnetic recording medium according to any one of claims 1 to 3.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP7697690A JPH03278315A (en) | 1990-03-28 | 1990-03-28 | Magnetic recording medium |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP7697690A JPH03278315A (en) | 1990-03-28 | 1990-03-28 | Magnetic recording medium |
Publications (1)
Publication Number | Publication Date |
---|---|
JPH03278315A true JPH03278315A (en) | 1991-12-10 |
Family
ID=13620818
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP7697690A Pending JPH03278315A (en) | 1990-03-28 | 1990-03-28 | Magnetic recording medium |
Country Status (1)
Country | Link |
---|---|
JP (1) | JPH03278315A (en) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2010248285A (en) * | 2009-04-10 | 2010-11-04 | Hitachi Maxell Ltd | Method for producing magnetic paint |
-
1990
- 1990-03-28 JP JP7697690A patent/JPH03278315A/en active Pending
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2010248285A (en) * | 2009-04-10 | 2010-11-04 | Hitachi Maxell Ltd | Method for producing magnetic paint |
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