JP7443055B2 - トナー - Google Patents
トナー Download PDFInfo
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- JP7443055B2 JP7443055B2 JP2019238249A JP2019238249A JP7443055B2 JP 7443055 B2 JP7443055 B2 JP 7443055B2 JP 2019238249 A JP2019238249 A JP 2019238249A JP 2019238249 A JP2019238249 A JP 2019238249A JP 7443055 B2 JP7443055 B2 JP 7443055B2
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- organosilicon polymer
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- 239000002245 particle Substances 0.000 claims description 136
- 229920001558 organosilicon polymer Polymers 0.000 claims description 72
- 239000000654 additive Substances 0.000 claims description 53
- 230000000996 additive effect Effects 0.000 claims description 41
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 118
- 239000010419 fine particle Substances 0.000 description 69
- 239000000377 silicon dioxide Substances 0.000 description 55
- 238000000034 method Methods 0.000 description 51
- 229920001577 copolymer Polymers 0.000 description 26
- 239000000178 monomer Substances 0.000 description 26
- 150000003961 organosilicon compounds Chemical class 0.000 description 24
- 229920005989 resin Polymers 0.000 description 23
- 239000011347 resin Substances 0.000 description 23
- 239000006185 dispersion Substances 0.000 description 21
- 239000000523 sample Substances 0.000 description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 20
- 239000000203 mixture Substances 0.000 description 18
- 238000002149 energy-dispersive X-ray emission spectroscopy Methods 0.000 description 17
- 238000004519 manufacturing process Methods 0.000 description 17
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- 238000006243 chemical reaction Methods 0.000 description 16
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- 238000005259 measurement Methods 0.000 description 16
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- 230000005494 condensation Effects 0.000 description 15
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- 239000003795 chemical substances by application Substances 0.000 description 13
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- 239000012736 aqueous medium Substances 0.000 description 12
- 229910052710 silicon Inorganic materials 0.000 description 12
- 238000006460 hydrolysis reaction Methods 0.000 description 11
- 238000006116 polymerization reaction Methods 0.000 description 11
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 10
- 125000004432 carbon atom Chemical group C* 0.000 description 9
- 150000001875 compounds Chemical class 0.000 description 9
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- 239000010703 silicon Substances 0.000 description 9
- 239000000243 solution Substances 0.000 description 9
- 238000003756 stirring Methods 0.000 description 9
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 8
- 238000005481 NMR spectroscopy Methods 0.000 description 8
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 7
- 239000003086 colorant Substances 0.000 description 7
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 description 7
- 239000011164 primary particle Substances 0.000 description 7
- 150000004756 silanes Chemical class 0.000 description 7
- 229910010271 silicon carbide Inorganic materials 0.000 description 7
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- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 description 6
- 229930006000 Sucrose Natural products 0.000 description 6
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 6
- 125000000217 alkyl group Chemical group 0.000 description 6
- 230000005540 biological transmission Effects 0.000 description 6
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- 238000000921 elemental analysis Methods 0.000 description 6
- 239000011521 glass Substances 0.000 description 6
- 239000007788 liquid Substances 0.000 description 6
- 239000003505 polymerization initiator Substances 0.000 description 6
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 6
- 239000005720 sucrose Substances 0.000 description 6
- 239000001993 wax Substances 0.000 description 6
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 description 5
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 5
- 239000007864 aqueous solution Substances 0.000 description 5
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- 238000000851 scanning transmission electron micrograph Methods 0.000 description 5
- 239000005049 silicon tetrachloride Substances 0.000 description 5
- MYRTYDVEIRVNKP-UHFFFAOYSA-N 1,2-Divinylbenzene Chemical compound C=CC1=CC=CC=C1C=C MYRTYDVEIRVNKP-UHFFFAOYSA-N 0.000 description 4
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 description 4
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 4
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 4
- 125000003545 alkoxy group Chemical group 0.000 description 4
- 125000004429 atom Chemical group 0.000 description 4
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 4
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 4
- 238000005119 centrifugation Methods 0.000 description 4
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- 239000006059 cover glass Substances 0.000 description 4
- 230000007774 longterm Effects 0.000 description 4
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
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- 239000002344 surface layer Substances 0.000 description 4
- 238000010558 suspension polymerization method Methods 0.000 description 4
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 3
- 239000006087 Silane Coupling Agent Substances 0.000 description 3
- 125000003668 acetyloxy group Chemical group [H]C([H])([H])C(=O)O[*] 0.000 description 3
- 239000003945 anionic surfactant Substances 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 3
- 238000006482 condensation reaction Methods 0.000 description 3
- 239000003431 cross linking reagent Substances 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 230000002209 hydrophobic effect Effects 0.000 description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 3
- 238000013507 mapping Methods 0.000 description 3
- 239000005055 methyl trichlorosilane Substances 0.000 description 3
- JLUFWMXJHAVVNN-UHFFFAOYSA-N methyltrichlorosilane Chemical compound C[Si](Cl)(Cl)Cl JLUFWMXJHAVVNN-UHFFFAOYSA-N 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 239000006082 mold release agent Substances 0.000 description 3
- 239000002736 nonionic surfactant Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 230000035484 reaction time Effects 0.000 description 3
- 229920006395 saturated elastomer Polymers 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 229910000077 silane Inorganic materials 0.000 description 3
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 description 3
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 3
- 229920002554 vinyl polymer Polymers 0.000 description 3
- UAJRSHJHFRVGMG-UHFFFAOYSA-N 1-ethenyl-4-methoxybenzene Chemical compound COC1=CC=C(C=C)C=C1 UAJRSHJHFRVGMG-UHFFFAOYSA-N 0.000 description 2
- 238000001644 13C nuclear magnetic resonance spectroscopy Methods 0.000 description 2
- LEJBBGNFPAFPKQ-UHFFFAOYSA-N 2-(2-prop-2-enoyloxyethoxy)ethyl prop-2-enoate Chemical compound C=CC(=O)OCCOCCOC(=O)C=C LEJBBGNFPAFPKQ-UHFFFAOYSA-N 0.000 description 2
- INQDDHNZXOAFFD-UHFFFAOYSA-N 2-[2-(2-prop-2-enoyloxyethoxy)ethoxy]ethyl prop-2-enoate Chemical compound C=CC(=O)OCCOCCOCCOC(=O)C=C INQDDHNZXOAFFD-UHFFFAOYSA-N 0.000 description 2
- HCLJOFJIQIJXHS-UHFFFAOYSA-N 2-[2-[2-(2-prop-2-enoyloxyethoxy)ethoxy]ethoxy]ethyl prop-2-enoate Chemical compound C=CC(=O)OCCOCCOCCOCCOC(=O)C=C HCLJOFJIQIJXHS-UHFFFAOYSA-N 0.000 description 2
- KUDUQBURMYMBIJ-UHFFFAOYSA-N 2-prop-2-enoyloxyethyl prop-2-enoate Chemical compound C=CC(=O)OCCOC(=O)C=C KUDUQBURMYMBIJ-UHFFFAOYSA-N 0.000 description 2
- SJECZPVISLOESU-UHFFFAOYSA-N 3-trimethoxysilylpropan-1-amine Chemical compound CO[Si](OC)(OC)CCCN SJECZPVISLOESU-UHFFFAOYSA-N 0.000 description 2
- RSWGJHLUYNHPMX-UHFFFAOYSA-N Abietic-Saeure Natural products C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- SOGAXMICEFXMKE-UHFFFAOYSA-N Butylmethacrylate Chemical compound CCCCOC(=O)C(C)=C SOGAXMICEFXMKE-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 description 2
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 description 2
- 239000004698 Polyethylene Substances 0.000 description 2
- 239000004743 Polypropylene Substances 0.000 description 2
- KHPCPRHQVVSZAH-HUOMCSJISA-N Rosin Natural products O(C/C=C/c1ccccc1)[C@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 KHPCPRHQVVSZAH-HUOMCSJISA-N 0.000 description 2
- 229920007962 Styrene Methyl Methacrylate Polymers 0.000 description 2
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 description 2
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
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- ORILYTVJVMAKLC-UHFFFAOYSA-N adamantane Chemical compound C1C(C2)CC3CC1CC2C3 ORILYTVJVMAKLC-UHFFFAOYSA-N 0.000 description 2
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- 125000001931 aliphatic group Chemical group 0.000 description 2
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- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 description 2
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 2
- XGZGKDQVCBHSGI-UHFFFAOYSA-N butyl(triethoxy)silane Chemical compound CCCC[Si](OCC)(OCC)OCC XGZGKDQVCBHSGI-UHFFFAOYSA-N 0.000 description 2
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- IJOOHPMOJXWVHK-UHFFFAOYSA-N chlorotrimethylsilane Chemical compound C[Si](C)(C)Cl IJOOHPMOJXWVHK-UHFFFAOYSA-N 0.000 description 2
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- 229910001882 dioxygen Inorganic materials 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- FJKIXWOMBXYWOQ-UHFFFAOYSA-N ethenoxyethane Chemical compound CCOC=C FJKIXWOMBXYWOQ-UHFFFAOYSA-N 0.000 description 2
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 2
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- 125000005843 halogen group Chemical group 0.000 description 2
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- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 description 2
- CZWLNMOIEMTDJY-UHFFFAOYSA-N hexyl(trimethoxy)silane Chemical compound CCCCCC[Si](OC)(OC)OC CZWLNMOIEMTDJY-UHFFFAOYSA-N 0.000 description 2
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- ADFPJHOAARPYLP-UHFFFAOYSA-N methyl 2-methylprop-2-enoate;styrene Chemical compound COC(=O)C(C)=C.C=CC1=CC=CC=C1 ADFPJHOAARPYLP-UHFFFAOYSA-N 0.000 description 2
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 description 2
- PHQOGHDTIVQXHL-UHFFFAOYSA-N n'-(3-trimethoxysilylpropyl)ethane-1,2-diamine Chemical compound CO[Si](OC)(OC)CCCNCCN PHQOGHDTIVQXHL-UHFFFAOYSA-N 0.000 description 2
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- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
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- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 2
- KHPCPRHQVVSZAH-UHFFFAOYSA-N trans-cinnamyl beta-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OCC=CC1=CC=CC=C1 KHPCPRHQVVSZAH-UHFFFAOYSA-N 0.000 description 2
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- WUMSTCDLAYQDNO-UHFFFAOYSA-N triethoxy(hexyl)silane Chemical compound CCCCCC[Si](OCC)(OCC)OCC WUMSTCDLAYQDNO-UHFFFAOYSA-N 0.000 description 2
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- ZNOCGWVLWPVKAO-UHFFFAOYSA-N trimethoxy(phenyl)silane Chemical compound CO[Si](OC)(OC)C1=CC=CC=C1 ZNOCGWVLWPVKAO-UHFFFAOYSA-N 0.000 description 2
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- KOZCZZVUFDCZGG-UHFFFAOYSA-N vinyl benzoate Chemical compound C=COC(=O)C1=CC=CC=C1 KOZCZZVUFDCZGG-UHFFFAOYSA-N 0.000 description 2
- SNOYUTZWILESAI-UHFFFAOYSA-N vinyl isopropyl ketone Natural products CC(C)C(=O)C=C SNOYUTZWILESAI-UHFFFAOYSA-N 0.000 description 2
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- KTLAPEGYFQVVFE-UHFFFAOYSA-N (1-acetyloxy-2-methylsilyloxyethyl) acetate Chemical compound C[SiH2]OCC(OC(C)=O)OC(C)=O KTLAPEGYFQVVFE-UHFFFAOYSA-N 0.000 description 1
- BOOBDAVNHSOIDB-UHFFFAOYSA-N (2,3-dichlorobenzoyl) 2,3-dichlorobenzenecarboperoxoate Chemical compound ClC1=CC=CC(C(=O)OOC(=O)C=2C(=C(Cl)C=CC=2)Cl)=C1Cl BOOBDAVNHSOIDB-UHFFFAOYSA-N 0.000 description 1
- BQCIDUSAKPWEOX-UHFFFAOYSA-N 1,1-Difluoroethene Chemical compound FC(F)=C BQCIDUSAKPWEOX-UHFFFAOYSA-N 0.000 description 1
- KOMNUTZXSVSERR-UHFFFAOYSA-N 1,3,5-tris(prop-2-enyl)-1,3,5-triazinane-2,4,6-trione Chemical compound C=CCN1C(=O)N(CC=C)C(=O)N(CC=C)C1=O KOMNUTZXSVSERR-UHFFFAOYSA-N 0.000 description 1
- YQJPWWLJDNCSCN-UHFFFAOYSA-N 1,3-diphenyltetramethyldisiloxane Chemical compound C=1C=CC=CC=1[Si](C)(C)O[Si](C)(C)C1=CC=CC=C1 YQJPWWLJDNCSCN-UHFFFAOYSA-N 0.000 description 1
- QOVCUELHTLHMEN-UHFFFAOYSA-N 1-butyl-4-ethenylbenzene Chemical compound CCCCC1=CC=C(C=C)C=C1 QOVCUELHTLHMEN-UHFFFAOYSA-N 0.000 description 1
- OZCMOJQQLBXBKI-UHFFFAOYSA-N 1-ethenoxy-2-methylpropane Chemical compound CC(C)COC=C OZCMOJQQLBXBKI-UHFFFAOYSA-N 0.000 description 1
- OEVVKKAVYQFQNV-UHFFFAOYSA-N 1-ethenyl-2,4-dimethylbenzene Chemical compound CC1=CC=C(C=C)C(C)=C1 OEVVKKAVYQFQNV-UHFFFAOYSA-N 0.000 description 1
- NVZWEEGUWXZOKI-UHFFFAOYSA-N 1-ethenyl-2-methylbenzene Chemical compound CC1=CC=CC=C1C=C NVZWEEGUWXZOKI-UHFFFAOYSA-N 0.000 description 1
- JZHGRUMIRATHIU-UHFFFAOYSA-N 1-ethenyl-3-methylbenzene Chemical compound CC1=CC=CC(C=C)=C1 JZHGRUMIRATHIU-UHFFFAOYSA-N 0.000 description 1
- QEDJMOONZLUIMC-UHFFFAOYSA-N 1-tert-butyl-4-ethenylbenzene Chemical compound CC(C)(C)C1=CC=C(C=C)C=C1 QEDJMOONZLUIMC-UHFFFAOYSA-N 0.000 description 1
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- MWZATVIRTOMCCI-UHFFFAOYSA-N trimethoxy-(2-methylphenyl)silane Chemical compound CO[Si](OC)(OC)C1=CC=CC=C1C MWZATVIRTOMCCI-UHFFFAOYSA-N 0.000 description 1
- XQEGZYAXBCFSBS-UHFFFAOYSA-N trimethoxy-(4-methylphenyl)silane Chemical compound CO[Si](OC)(OC)C1=CC=C(C)C=C1 XQEGZYAXBCFSBS-UHFFFAOYSA-N 0.000 description 1
- KHOQXNHADJBILQ-UHFFFAOYSA-N trimethyl(sulfanyl)silane Chemical compound C[Si](C)(C)S KHOQXNHADJBILQ-UHFFFAOYSA-N 0.000 description 1
- 239000005051 trimethylchlorosilane Substances 0.000 description 1
- PQDJYEQOELDLCP-UHFFFAOYSA-N trimethylsilane Chemical compound C[SiH](C)C PQDJYEQOELDLCP-UHFFFAOYSA-N 0.000 description 1
- GRPURDFRFHUDSP-UHFFFAOYSA-N tris(prop-2-enyl) benzene-1,2,4-tricarboxylate Chemical compound C=CCOC(=O)C1=CC=C(C(=O)OCC=C)C(C(=O)OCC=C)=C1 GRPURDFRFHUDSP-UHFFFAOYSA-N 0.000 description 1
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
- 239000012178 vegetable wax Substances 0.000 description 1
- FUSUHKVFWTUUBE-UHFFFAOYSA-N vinyl methyl ketone Natural products CC(=O)C=C FUSUHKVFWTUUBE-UHFFFAOYSA-N 0.000 description 1
- UKRDPEFKFJNXQM-UHFFFAOYSA-N vinylsilane Chemical class [SiH3]C=C UKRDPEFKFJNXQM-UHFFFAOYSA-N 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
- LRXTYHSAJDENHV-UHFFFAOYSA-H zinc phosphate Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O LRXTYHSAJDENHV-UHFFFAOYSA-H 0.000 description 1
- 229910000165 zinc phosphate Inorganic materials 0.000 description 1
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 description 1
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Description
これまで、長寿命化及び高画質化を目指して、トナー粒子の表層には様々な外添剤が利用されてきた。しかし、特に長寿命化した本体においては、長期にわたる画像出力によって、外添剤の移動・脱離・埋没といった耐久変化が起こり、初期の高画質を維持することが難しいという課題がある。
こうした課題の解決のために、外添以外の手法で耐久変化を抑制するために、R-Si(O1/2)3で表される部分構造を有する有機ケイ素重合体でトナー粒子表層を覆う提案が成されている(特許文献1)。これは、湿式においてトナー表層を化学的な架橋によって覆っているため、耐久変化が少ないという特徴がある。この有機ケイ素重合体の構造に関しては検討が進んでおり、表層の有機ケイ素重合体の凸部を大きくすることで、現像効率を向上させることが分かっている。
本発明の目的は、表面に有機ケイ素重合体の凸部を有するトナーに対し、現像効率に優れるとともに、ベタ画像やハーフトーン画像の均一性の高いトナーを提供することにある。
該トナー粒子は、その表面に該有機ケイ素重合体で形成された凸部を有しており、
該トナー粒子のTEMによる断面観察によって、該トナー粒子を観察した際、該凸部の該トナー粒子との連続した界面における最大の線分を凸幅Wとし、該凸幅Wの法線方向の該凸部の最大長を凸径Dとし、該凸径Dと重なる凸幅Wまでの長さを凸高さHとしたとき、該凸高さHは30nm以上300nm以下の範囲であり、該凸幅Wと該凸径Dの比D/Wが0.33以上0.80以下であり、
外添剤Aは、下記式(1)で表される稠密度が0.40以上0.80以下であることを特徴とするトナーに関する。
稠密度=外添剤Aの面積/外添剤Aの包絡線により囲まれた領域の面積 (1)
稠密度=外添剤Aの面積/外添剤Aの包絡線により囲まれた領域の面積 (1)
SiCl4+2H2+O2→SiO2+4HCl
(1)流動性付与剤:アルミナ微粒子、酸化チタン微粒子、カーボンブラック及びフッ化カーボン。
(2)研磨剤:金属酸化物の微粒子(チタン酸ストロンチウム、酸化セリウム、アルミナ、酸化マグネシウム、及び酸化クロムなどの微粒子)、窒化物の微粒子(窒化ケイ素などの微粒子)、炭化物の微粒子(炭化ケイ素などの微粒子)、金属塩の微粒子(硫酸カルシウム、硫酸バリウム、及び炭酸カルシウムなどの微粒子)。
(3)滑剤:フッ素系樹脂の微粒子(フッ化ビニリデン、ポリテトラフルオロエチレンなどの微粒子)、脂肪酸金属塩の微粒子(ステアリン酸亜鉛、ステアリン酸カルシウムなどの微粒子)。
(4)荷電制御性微粒子:金属酸化物の微粒子(酸化錫、酸化チタン、酸化亜鉛、及びアルミナなどの微粒子)、カーボンブラック。
走査透過型電子顕微鏡(STEM)で観察されるトナーの断面は以下のようにして作製する。
上記走査透過型電子顕微鏡(STEM)を用いたトナーの断面のSTEM画像において、凸高さHが30nm以上300nm以下である凸部に対し、該凸高さHの累積分布をとり、該凸高さHの小さい方から積算して80個数%にあたる該凸高さをH80(単位:nm)とする。
明部面積の面積割合は、走査電子顕微鏡を用いて、トナーの表面観察を行う。そして、トナー表面の1.5μm四方の反射電子像を取得し、該反射電子像中の有機ケイ素重合体部分が明部となるように二値化処理した画像を得、該画像の全面積に対する該画像の明部面積の割合を求める。
使用装置:カールツァイスマイクロスコピー株式会社製 ULTRA PLUS
加速電圧:1.0kV
WD:2.0mm
Aperture Size:30.0μm
検出信号:EsB(エネルギー選択式反射電子)
EsB Grid:800V
観察倍率:50,000倍
コントラスト:63.0±5.0%(参考値)
ブライトネス:38.0±5.0%(参考値)
解像度:1024×768
前処理:トナー粒子をカーボンテープに散布(蒸着は行わない)
SEM/EDSの装置及び観察条件は、下記の通りである。
使用装置(SEM):カールツァイスマイクロスコピー株式会社製 ULTRA PLUS
使用装置(EDS):サーモフィッシャーサイエンティフィック株式会社製 NORAN System 7、Ultra Dry EDS Detecter
加速電圧:5.0kV
WD:7.0mm
Aperture Size:30.0μm
検出信号:SE2(二次電子)
観察倍率:50,000倍
モード:Spectral Imaging
前処理:トナー粒子をカーボンテープに散布し、白金スパッタ
本手法で取得したケイ素元素のマッピング像と、前記反射電子像を重ね合わせ、マッピング像のケイ素原子部と反射電子像の明部とが一致することを確認する。
有機ケイ素重合体の同定方法は走査型電子顕微鏡(SEM)による観察及びエネルギー分散型X線分析(EDS)による元素分析を組み合わせて行う。
走査型電子顕微鏡「日立超高分解能電界放出形走査電子顕微鏡 S-4800」((株)日立ハイテクノロジーズ)及びエネルギー分散型X線分析(EDS)による元素分析を組み合わせて行う。
トナー中に含まれる有機ケイ素重合体の構成化合物の組成と比率の同定には、NMRを用いる。
超音波処理装置:超音波式ホモジナイザーVP-050(タイテック株式会社製)
マイクロチップ:ステップ型マイクロチップ、先端径φ2mm
マイクロチップの先端位置:ガラスバイアルの中央部、且つバイアル底面から5mmの高さ
超音波条件:強度30%、30分
装置:JEOLRESONANCE製JNM-ECX500II
試料管:3.2mmφ
試料:サンプル又は有機ケイ素重合体
測定温度:室温
パルスモード:CP/MAS
測定核周波数:123.25MHz(13C)
基準物質:アダマンタン(外部標準:29.5ppm)
試料回転数:20kHz
コンタクト時間:2ms
遅延時間:2s
積算回数:1024回
該方法にて、ケイ素原子に結合しているメチル基(Si-CH3)、エチル基(Si-C2H5)、プロピル基(Si-C3H7)、ブチル基(Si-C4H9)、ペンチル基(Si-C5H11)、ヘキシル基(Si-C6H13)又はフェニル基(Si-C6H5-)などに起因するシグナルの有無により、上記Rで表される炭化水素基を確認する。
装置:JNM-ECX5002 (JEOL RESONANCE)
温度:室温
測定法:DDMAS法 29Si 45°
試料管:ジルコニア3.2mmφ
試料:試験管に粉末状態で充填
試料回転数:10kHz
relaxation delay :180s
Scan:2000
該測定後に、サンプル又は有機ケイ素重合体の、置換基及び結合基の異なる複数のシラン成分をカーブフィティングにて下記X1構造、X2構造、X3構造、及びX4構造にピーク分離して、それぞれピーク面積を算出する。
X1構造:(Ri)(Rj)(Rk)SiO1/2 (A1)
X2構造:(Rg)(Rh)Si(O1/2)2 (A2)
X3構造:RmSi(O1/2)3 (A3)
X4構造:Si(O1/2)4 (A4)
トナーを、上記のようにクロロホルムに分散させ、その後に遠心分離を用い、比重の差で有機ケイ素重合体及びシリカ微粒子などの外添剤を分離し、各サンプルを得、有機ケイ素重合体又はシリカ微粒子などの外添剤の含有量を求める。
(水系媒体1の調製)
撹拌機、温度計、及び還流管を具備した反応容器に、イオン交換水650.0部及びリン酸ナトリウム(ラサ工業社製・12水和物)14.0部を投入し、窒素パージしながら65℃で1.0時間保温した。
・スチレン :60.0部
・C.I.ピグメントブルー15:3 : 6.5部
前記材料をアトライタ(三井三池化工機株式会社製)に投入し、さらに直径1.7mmのジルコニア粒子を用いて、220rpmで5.0時間分散させた後、ジルコニア粒子を取り除き、着色剤分散液を調製した。
・スチレン :20.0部
・n-ブチルアクリレート :20.0部
・架橋剤(ジビニルベンゼン) : 0.3部
・飽和ポリエステル樹脂 : 5.0部
(プロピレンオキサイド変性ビスフェノールA(2モル付加物)とテレフタル酸との重縮合物(モル比10:12)、ガラス転移温度(Tg)が68℃、重量平均分子量(Mw)が10000、分子量分布(Mw/Mn)が5.12)
・フィッシャートロプシュワックス(融点78℃) : 7.0部
該材料を上記着色剤分散液に加え、65℃に加熱後、T.K.ホモミクサー(特殊機化工業株式会社製)を用いて、500rpmで均一に溶解及び分散し、重合性単量体組成物を調製した。
水系媒体1の温度を70℃に調整し、T.K.ホモミクサーの回転数を15000rpmに保ちながら、水系媒体1中に重合性単量体組成物を投入し、重合開始剤であるt-ブチルパーオキシピバレート10.0部を添加した。そのまま、該撹拌装置にて15000rpmを維持しつつ10分間造粒した。
造粒工程の後、撹拌機をプロペラ撹拌羽根に換え150rpmで撹拌しながら70℃を保持して5.0時間重合を行い、さらに、85℃に昇温して2.0時間保持することで重合を行った。
撹拌機、温度計を備えた反応容器に、イオン交換水60.0部を秤量し、10質量%の塩酸を用いてpHを4.0に調整した。これを撹拌しながら加熱し、温度を40℃にした。その後、有機ケイ素化合物であるメチルトリエトキシシラン40.0部を添加して2時間以上撹拌して加水分解を行った。
有機ケイ素重合体の形成工程終了後、トナー粒子分散液を冷却し、トナー粒子分散液に塩酸を加えpHを1.5以下に調整して1.0時間、撹拌しながら放置した。その後、加圧ろ過器で固液分離し、トナーケーキを得た。
表1に示す条件に変更した以外は、トナー粒子1の製造例と同様にしてトナー粒子2~19及び比較トナー粒子2~5を得た。トナー粒子2~19及び比較2~5の製造条件を表1に示す。比較トナー粒子1は、この操作を実施しない。
外添剤A1~6及びA8は、以下のように製造した。
外添剤A7は、アルミナ、AKP-30(住友化学株式会社)を用いた。表2に外添剤A7の物性を示す。
ジャケット内に7℃の水を通水したヘンシェルミキサ(日本コークス工業株式会社製 FM10C型)中に100.00部のトナー粒子1、及び、1.00部の外添剤A1を投入した。次に、該ジャケット内の水温が7℃±1℃で安定してから、回転羽根の周速を38m/secとして10分間混合した。該混合において、ヘンシェルミキサの槽内温度が25℃を超えないようジャケット内の通水量を適宜調整した。
表3に示す外添剤Aに変更し、ヘンシェルミキサによる外添条件を適宜変更した以外は、トナー1の製造例と同様にしてトナー2~19及び比較トナー1~5を得た。トナー2~19及び比較トナー1~5の製造条件及び物性を表3に示す。
トナー1について下記評価を行った。結果は表4に示す。
評価機として、市販のキヤノン製レーザービームプリンタLBP7700Cの改造機を用いた。改造点は、評価機本体及びソフトウェアを変更することにより、現像ローラーの回転速度が360mm/secとなるようにした。
(評価基準)
A:画像濃度にムラがなく均一である。
B:画像濃度に軽微なムラがあるが、使用上問題とならないレベル。
C:画像濃度にムラがあるが、使用上問題とならないレベル。
D:画像濃度にムラがあり、均一なベタ画像になっていないレベル。
評価機として、市販のキヤノン製レーザービームプリンタLBP7700Cの改造機を用いた。改造点は、評価機本体及びソフトウェアを変更することにより、現像ローラーの回転速度が360mm/secとなるようにした。
(初期評価基準)
A:画像濃度にムラがなく均一である。
B:画像濃度に軽微なムラがあるが、使用上問題とならないレベル。
C:画像濃度にムラがあるが、使用上問題とならないレベル。
D:画像濃度にムラがあり、均一なベタ画像になっていないレベル。
(10000枚目評価基準)
A:画像濃度にムラがなく均一である。
B:画像濃度に軽微なムラがあるが、使用上問題とならないレベル。
C:画像濃度にムラがあるが、使用上問題とならないレベル。
D:画像濃度にムラがあり、均一なベタ画像になっていないレベル。
評価機として、市販のキヤノン製レーザービームプリンタLBP7700Cの改造機を用いた。改造点は、評価機本体及びソフトウェアを変更することにより、現像ローラーの回転速度が360mm/secとなるようにした。
(評価基準)
A:ゴースト未発生。
B:ゴーストがごく軽微に発生。
C:ゴーストが軽微に発生。
D:ゴーストが顕著に発生。
実施例1において、トナー1を、トナー2~19、及び、比較トナー1~5に変更すること以外は同様にして、評価を実施した。結果は表4に示す。
Claims (4)
- 表面に有機ケイ素重合体を有するトナー粒子と、外添剤Aとを有するトナーであって、
該トナー粒子は、その表面に該有機ケイ素重合体で形成された凸部を有しており、
該トナー粒子のTEMによる断面観察によって、該トナー粒子を観察した際、該凸部の該トナー粒子との連続した界面における最大の線分を凸幅Wとし、該凸幅Wの法線方向の該凸部の最大長を凸径Dとし、該凸径Dと重なる凸幅Wまでの長さを凸高さHとしたとき、該凸高さHは30nm以上300nm以下の範囲であり、該凸幅Wと該凸径Dの比D/Wが0.33以上0.80以下であり、
外添剤Aは、下記式(1)で表される稠密度が0.40以上0.80以下である
ことを特徴とするトナー。
稠密度=外添剤Aの面積/外添剤Aの包絡線により囲まれた領域の面積 (1) - 前記外添剤Aの包絡線の長軸が50nm以上500nm以下である請求項1のトナー。
- 前記トナーは、前記外添剤Aを前記トナー100質量部に対して0.05質量部以上3.00質量部以下有する請求項1または2のトナー。
- 前記トナーの表面積をSとし、前記凸幅Wの総和をΣWとしたとき、下記式(2)を満たす請求項1~3のいずれか1項に記載のトナー。
0.20nm-1<ΣW/S<0.70nm-1 (2)
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JP2019124854A (ja) | 2018-01-18 | 2019-07-25 | 株式会社リコー | トナー、トナー収容ユニット、及び画像形成装置 |
JP2019191451A (ja) | 2018-04-27 | 2019-10-31 | キヤノン株式会社 | トナー |
JP2019211774A (ja) | 2018-05-31 | 2019-12-12 | キヤノン株式会社 | 画像形成装置及び画像形成方法 |
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