JPH04333055A - Production of toner - Google Patents
Production of tonerInfo
- Publication number
- JPH04333055A JPH04333055A JP3102541A JP10254191A JPH04333055A JP H04333055 A JPH04333055 A JP H04333055A JP 3102541 A JP3102541 A JP 3102541A JP 10254191 A JP10254191 A JP 10254191A JP H04333055 A JPH04333055 A JP H04333055A
- Authority
- JP
- Japan
- Prior art keywords
- resin
- particles
- fine particles
- toner
- inner core
- 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
- 238000004519 manufacturing process Methods 0.000 title claims description 13
- 229920005989 resin Polymers 0.000 claims abstract description 93
- 239000011347 resin Substances 0.000 claims abstract description 93
- 239000002245 particle Substances 0.000 claims abstract description 64
- 239000010419 fine particle Substances 0.000 claims abstract description 60
- 238000000034 method Methods 0.000 claims abstract description 51
- 239000007771 core particle Substances 0.000 claims abstract description 42
- 239000002904 solvent Substances 0.000 claims abstract description 22
- 239000011247 coating layer Substances 0.000 claims abstract description 15
- 239000003086 colorant Substances 0.000 claims abstract description 11
- 239000011230 binding agent Substances 0.000 claims abstract description 9
- 238000011161 development Methods 0.000 claims description 15
- 239000010954 inorganic particle Substances 0.000 claims description 10
- 239000000758 substrate Substances 0.000 claims 1
- 239000000203 mixture Substances 0.000 abstract description 14
- 238000001694 spray drying Methods 0.000 abstract description 6
- 239000000463 material Substances 0.000 abstract description 5
- 238000004898 kneading Methods 0.000 abstract description 3
- 238000010298 pulverizing process Methods 0.000 abstract description 2
- 238000000151 deposition Methods 0.000 abstract 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 46
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 40
- 229920001577 copolymer Polymers 0.000 description 29
- 239000000377 silicon dioxide Substances 0.000 description 22
- 229910052681 coesite Inorganic materials 0.000 description 21
- 229910052906 cristobalite Inorganic materials 0.000 description 21
- 229910052682 stishovite Inorganic materials 0.000 description 21
- 229910052905 tridymite Inorganic materials 0.000 description 21
- 235000012239 silicon dioxide Nutrition 0.000 description 20
- 238000011282 treatment Methods 0.000 description 19
- 239000006185 dispersion Substances 0.000 description 14
- 239000001993 wax Substances 0.000 description 14
- 229920001490 poly(butyl methacrylate) polymer Polymers 0.000 description 13
- -1 isobutyl maleic acid Chemical compound 0.000 description 9
- 239000000126 substance Substances 0.000 description 8
- 239000000843 powder Substances 0.000 description 7
- 239000003795 chemical substances by application Substances 0.000 description 6
- SOGAXMICEFXMKE-UHFFFAOYSA-N alpha-Methyl-n-butyl acrylate Natural products CCCCOC(=O)C(C)=C SOGAXMICEFXMKE-UHFFFAOYSA-N 0.000 description 5
- 230000000903 blocking effect Effects 0.000 description 5
- MTAZNLWOLGHBHU-UHFFFAOYSA-N butadiene-styrene rubber Chemical compound C=CC=C.C=CC1=CC=CC=C1 MTAZNLWOLGHBHU-UHFFFAOYSA-N 0.000 description 5
- 239000007822 coupling agent Substances 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- 230000002776 aggregation Effects 0.000 description 4
- 239000006229 carbon black Substances 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 239000012188 paraffin wax Substances 0.000 description 4
- 235000019271 petrolatum Nutrition 0.000 description 4
- 239000007921 spray Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 description 3
- 239000004698 Polyethylene Substances 0.000 description 3
- 239000004743 Polypropylene Substances 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 238000011109 contamination Methods 0.000 description 3
- 230000006866 deterioration Effects 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 239000006247 magnetic powder Substances 0.000 description 3
- 108091008695 photoreceptors Proteins 0.000 description 3
- 239000000049 pigment Substances 0.000 description 3
- 229920000728 polyester Polymers 0.000 description 3
- 229920000573 polyethylene Polymers 0.000 description 3
- 229920001155 polypropylene Polymers 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000001238 wet grinding Methods 0.000 description 3
- 239000004925 Acrylic resin Substances 0.000 description 2
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 description 2
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 150000007513 acids Chemical class 0.000 description 2
- 229920006243 acrylic copolymer Polymers 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 238000004220 aggregation Methods 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 description 2
- 239000004203 carnauba wax Substances 0.000 description 2
- 235000013869 carnauba wax Nutrition 0.000 description 2
- 239000004359 castor oil Substances 0.000 description 2
- 235000019438 castor oil Nutrition 0.000 description 2
- 229910052804 chromium Inorganic materials 0.000 description 2
- 239000011651 chromium Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 125000001664 diethylamino group Chemical group [H]C([H])([H])C([H])([H])N(*)C([H])([H])C([H])([H])[H] 0.000 description 2
- 239000002270 dispersing agent Substances 0.000 description 2
- 239000000975 dye Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000003822 epoxy resin Substances 0.000 description 2
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 2
- 125000000524 functional group Chemical group 0.000 description 2
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 description 2
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000011976 maleic acid Substances 0.000 description 2
- 239000011812 mixed powder Substances 0.000 description 2
- 239000012170 montan wax Substances 0.000 description 2
- 229920000647 polyepoxide Polymers 0.000 description 2
- 229920005990 polystyrene resin Polymers 0.000 description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 229920002050 silicone resin Polymers 0.000 description 2
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 2
- DSEKYWAQQVUQTP-XEWMWGOFSA-N (2r,4r,4as,6as,6as,6br,8ar,12ar,14as,14bs)-2-hydroxy-4,4a,6a,6b,8a,11,11,14a-octamethyl-2,4,5,6,6a,7,8,9,10,12,12a,13,14,14b-tetradecahydro-1h-picen-3-one Chemical compound C([C@H]1[C@]2(C)CC[C@@]34C)C(C)(C)CC[C@]1(C)CC[C@]2(C)[C@H]4CC[C@@]1(C)[C@H]3C[C@@H](O)C(=O)[C@@H]1C DSEKYWAQQVUQTP-XEWMWGOFSA-N 0.000 description 1
- 229920002818 (Hydroxyethyl)methacrylate Polymers 0.000 description 1
- BQCIDUSAKPWEOX-UHFFFAOYSA-N 1,1-Difluoroethene Chemical compound FC(F)=C BQCIDUSAKPWEOX-UHFFFAOYSA-N 0.000 description 1
- VBICKXHEKHSIBG-UHFFFAOYSA-N 1-monostearoylglycerol Chemical compound CCCCCCCCCCCCCCCCCC(=O)OCC(O)CO VBICKXHEKHSIBG-UHFFFAOYSA-N 0.000 description 1
- ZNQVEEAIQZEUHB-UHFFFAOYSA-N 2-ethoxyethanol Chemical compound CCOCCO ZNQVEEAIQZEUHB-UHFFFAOYSA-N 0.000 description 1
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 description 1
- 229920002126 Acrylic acid copolymer Polymers 0.000 description 1
- 229920000178 Acrylic resin Polymers 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- 229920000089 Cyclic olefin copolymer Polymers 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- 239000004716 Ethylene/acrylic acid copolymer Substances 0.000 description 1
- DCXXMTOCNZCJGO-UHFFFAOYSA-N Glycerol trioctadecanoate Natural products CCCCCCCCCCCCCCCCCC(=O)OCC(OC(=O)CCCCCCCCCCCCCCCCC)COC(=O)CCCCCCCCCCCCCCCCC DCXXMTOCNZCJGO-UHFFFAOYSA-N 0.000 description 1
- 239000004166 Lanolin Substances 0.000 description 1
- JHWNWJKBPDFINM-UHFFFAOYSA-N Laurolactam Chemical compound O=C1CCCCCCCCCCCN1 JHWNWJKBPDFINM-UHFFFAOYSA-N 0.000 description 1
- 229920000877 Melamine resin Polymers 0.000 description 1
- 239000004640 Melamine resin Substances 0.000 description 1
- CERQOIWHTDAKMF-UHFFFAOYSA-M Methacrylate Chemical compound CC(=C)C([O-])=O CERQOIWHTDAKMF-UHFFFAOYSA-M 0.000 description 1
- 229920000571 Nylon 11 Polymers 0.000 description 1
- 229920000299 Nylon 12 Polymers 0.000 description 1
- 229920002302 Nylon 6,6 Polymers 0.000 description 1
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 235000021314 Palmitic acid Nutrition 0.000 description 1
- 239000004264 Petrolatum Substances 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 1
- 239000005062 Polybutadiene Substances 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 239000004793 Polystyrene Substances 0.000 description 1
- NRCMAYZCPIVABH-UHFFFAOYSA-N Quinacridone Chemical compound N1C2=CC=CC=C2C(=O)C2=C1C=C1C(=O)C3=CC=CC=C3NC1=C2 NRCMAYZCPIVABH-UHFFFAOYSA-N 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- 229910010059 TiBaO3 Inorganic materials 0.000 description 1
- 229910010282 TiON Inorganic materials 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 229920006322 acrylamide copolymer Polymers 0.000 description 1
- 125000005396 acrylic acid ester group Chemical group 0.000 description 1
- 229920002877 acrylic styrene acrylonitrile Polymers 0.000 description 1
- 229920000122 acrylonitrile butadiene styrene Polymers 0.000 description 1
- 238000011276 addition treatment Methods 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 235000013871 bee wax Nutrition 0.000 description 1
- 239000012166 beeswax Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- DFYKHEXCUQCPEB-UHFFFAOYSA-N butyl 2-methylprop-2-enoate;styrene Chemical compound C=CC1=CC=CC=C1.CCCCOC(=O)C(C)=C DFYKHEXCUQCPEB-UHFFFAOYSA-N 0.000 description 1
- 239000004204 candelilla wax Substances 0.000 description 1
- 235000013868 candelilla wax Nutrition 0.000 description 1
- 229940073532 candelilla wax Drugs 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 229910052570 clay Inorganic materials 0.000 description 1
- 238000004581 coalescence Methods 0.000 description 1
- 239000006258 conductive agent Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 229920006037 cross link polymer Polymers 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- MYRTYDVEIRVNKP-UHFFFAOYSA-N divinylbenzene Substances C=CC1=CC=CC=C1C=C MYRTYDVEIRVNKP-UHFFFAOYSA-N 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- QHZOMAXECYYXGP-UHFFFAOYSA-N ethene;prop-2-enoic acid Chemical compound C=C.OC(=O)C=C QHZOMAXECYYXGP-UHFFFAOYSA-N 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- NBVXSUQYWXRMNV-UHFFFAOYSA-N fluoromethane Chemical compound FC NBVXSUQYWXRMNV-UHFFFAOYSA-N 0.000 description 1
- 230000009477 glass transition Effects 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- LNEPOXFFQSENCJ-UHFFFAOYSA-N haloperidol Chemical compound C1CC(O)(C=2C=CC(Cl)=CC=2)CCN1CCCC(=O)C1=CC=C(F)C=C1 LNEPOXFFQSENCJ-UHFFFAOYSA-N 0.000 description 1
- IUJAMGNYPWYUPM-UHFFFAOYSA-N hentriacontane Chemical compound CCCCCCCCCCCCCCCCCCCCCCCCCCCCCCC IUJAMGNYPWYUPM-UHFFFAOYSA-N 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 230000009191 jumping Effects 0.000 description 1
- 235000019388 lanolin Nutrition 0.000 description 1
- 229940039717 lanolin Drugs 0.000 description 1
- HYLDLLCHFLSKAG-UHFFFAOYSA-M lissamine flavine FF Chemical compound [Na+].C1=CC(C)=CC=C1N(C1=O)C(=O)C2=C3C1=CC=CC3=C(N)C(S([O-])(=O)=O)=C2 HYLDLLCHFLSKAG-UHFFFAOYSA-M 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000010445 mica Substances 0.000 description 1
- 229910052618 mica group Inorganic materials 0.000 description 1
- 239000004200 microcrystalline wax Substances 0.000 description 1
- 235000019808 microcrystalline wax Nutrition 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- LSWADWIFYOAQRZ-UHFFFAOYSA-N n-(ethoxymethyl)prop-2-enamide Chemical compound CCOCNC(=O)C=C LSWADWIFYOAQRZ-UHFFFAOYSA-N 0.000 description 1
- WQEPLUUGTLDZJY-UHFFFAOYSA-N n-Pentadecanoic acid Natural products CCCCCCCCCCCCCCC(O)=O WQEPLUUGTLDZJY-UHFFFAOYSA-N 0.000 description 1
- 125000004108 n-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- GNRSAWUEBMWBQH-UHFFFAOYSA-N nickel(II) oxide Inorganic materials [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 235000019809 paraffin wax Nutrition 0.000 description 1
- 229940066842 petrolatum Drugs 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
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- IEQIEDJGQAUEQZ-UHFFFAOYSA-N phthalocyanine Chemical compound N1C(N=C2C3=CC=CC=C3C(N=C3C4=CC=CC=C4C(=N4)N3)=N2)=C(C=CC=C2)C2=C1N=C1C2=CC=CC=C2C4=N1 IEQIEDJGQAUEQZ-UHFFFAOYSA-N 0.000 description 1
- 229920001483 poly(ethyl methacrylate) polymer Polymers 0.000 description 1
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 1
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 description 1
- 108700004370 poly-gamma-methylglutamate Proteins 0.000 description 1
- 229920006122 polyamide resin Polymers 0.000 description 1
- 229920002857 polybutadiene Polymers 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 229920013716 polyethylene resin Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- 239000004926 polymethyl methacrylate Substances 0.000 description 1
- 229920000098 polyolefin Polymers 0.000 description 1
- 229920005672 polyolefin resin Polymers 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 229920005749 polyurethane resin Polymers 0.000 description 1
- 229920002689 polyvinyl acetate Polymers 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004076 pyridyl group Chemical group 0.000 description 1
- 150000003242 quaternary ammonium salts Chemical class 0.000 description 1
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 1
- 229940043267 rhodamine b Drugs 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- DCVWZWOEQMSMLR-UHFFFAOYSA-N silylperoxysilane Chemical compound [SiH3]OO[SiH3] DCVWZWOEQMSMLR-UHFFFAOYSA-N 0.000 description 1
- 239000000344 soap Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 229920003048 styrene butadiene rubber Polymers 0.000 description 1
- 150000003440 styrenes Chemical class 0.000 description 1
- 229940124530 sulfonamide Drugs 0.000 description 1
- 150000003456 sulfonamides Chemical class 0.000 description 1
- 239000000454 talc Substances 0.000 description 1
- 229910052623 talc Inorganic materials 0.000 description 1
- QHGNHLZPVBIIPX-UHFFFAOYSA-N tin(II) oxide Inorganic materials [Sn]=O QHGNHLZPVBIIPX-UHFFFAOYSA-N 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
- XLOMVQKBTHCTTD-UHFFFAOYSA-N zinc oxide Inorganic materials [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 1
Abstract
Description
【０００１】0001
【産業上の利用分野】本発明は、電子写真法などに使用
されている乾式現像用トナーに関する。詳しくは、多層
構造を有するトナーに関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a dry developing toner used in electrophotography and the like. Specifically, the present invention relates to a toner having a multilayer structure.
【０００２】0002
【従来の技術】従来、電子写真法としては、米国特許第
２２９７６９１に示させているカールソンプロセスを基
本として、これまでに多数の方法が提案されている。一
般には光導電性物質を用いた感光体上に静電気的潜像を
形成し、次に前記潜像に‘トナー’と呼ばれる微粉末を
選択的に付着させ、現像を行い前記潜像を顕像化する。
この顕像化したトナーを必要に応じて紙などの転写材に
転写した後、熱及び圧力、または溶剤蒸気などにより定
着し画像形成物を得るものである。2. Description of the Related Art Conventionally, as an electrophotographic method, many methods have been proposed based on the Carlson process shown in US Pat. No. 2,297,691. Generally, an electrostatic latent image is formed on a photoreceptor using a photoconductive substance, and then a fine powder called 'toner' is selectively attached to the latent image, and development is performed to make the latent image visible. become The visualized toner is transferred to a transfer material such as paper if necessary, and then fixed by heat and pressure, solvent vapor, etc. to obtain an image-formed product.
【０００３】現像方法としては乾式現像方式、液体現像
方式に大別できる。さらに乾式現像方式としてはキャリ
アを使用する二成分現像方式として磁気ブラシ現像法、
カスケード現像法などが知られていて、また、一成分現
像方式としては、ジャンピング現像法、ＦＥＥＤ現像法
、磁気ブラシ現像法などが知られている。これらの現像
方式に使用されるトナーは、さらに絶縁性と導電性に分
類される。一般にこれらの現像方法に使用されるトナー
は樹脂中に染料、顔料などの着色剤、帯電制御剤などを
分散させた約１０μｍの微粒子の表面に種種の物質を付
着させたものが使用されている。しかし、これらの微粉
末を前記の現像方法に用いるためには種種の物理的化学
的特性が要求される。要求される現像剤の特性としては
、おもに粒径・帯電性・電気抵抗・磁気特性・凝集性・
流動性等があり、改良がなされている。なかでもトナー
搬送に影響を与える凝集性、流動性についてはこれまで
に多数の提案がなされており、例えばシリカ粉末をトナ
ーの表面に付着させることにより流動性を向上させるこ
とが一般に知られている。[0003] Developing methods can be roughly divided into dry developing methods and liquid developing methods. Furthermore, as a dry development method, a magnetic brush development method is used as a two-component development method that uses a carrier.
A cascade development method is known, and a jumping development method, a FEED development method, a magnetic brush development method, etc. are known as one-component development methods. The toners used in these development methods are further classified into insulating and conductive toners. Generally, the toner used in these developing methods is made by dispersing colorants such as dyes and pigments, charge control agents, etc. in resin, and having various substances adhered to the surface of fine particles of approximately 10 μm. . However, in order to use these fine powders in the above-mentioned development method, various physical and chemical properties are required. The required developer properties are mainly particle size, chargeability, electrical resistance, magnetic properties, cohesiveness,
It has good fluidity and has been improved. Among these, many proposals have been made to date regarding cohesiveness and fluidity, which affect toner transport. For example, it is generally known that fluidity can be improved by attaching silica powder to the surface of toner. .
【０００４】トナー表面に種種の物質を付着させる方法
としては、流動乾燥炉などを使用して熱により付着させ
る方法、ボールミルなどの混合機を用いて機械的な力に
より付着させる方法などが知られている。また、噴霧乾
燥方法、噴霧造粒方法などがある。他には、高速ジェッ
ト気流により分散すると同時に、処理剤と接触させる方
法（平２−４２４５２）等も提案されている。[0004] Known methods for attaching various substances to the toner surface include a method in which the substances are attached by heat using a fluidized drying oven, and a method in which the substances are attached by mechanical force using a mixer such as a ball mill. ing. Further, there are a spray drying method, a spray granulation method, and the like. Other proposals include a method of dispersing by a high-speed jet stream and simultaneously contacting with a processing agent (Hei 2-42452).
【０００５】[0005]
【発明が解決しようとする課題】しかしながら、前述の
付着方法では、表面に付着した微粒子の付着力が弱く、
トナー搬送時及び現像時にトナー表面から剥がれてしま
い使用雰囲気温度によって容易に凝集が起こり、ブロッ
キングやケーキングによりトナーの現像特性が低下する
という欠点を有している。さらに剥がれた微粒子により
装置内汚染が生じ、画像劣化、機械故障などの悪影響を
及ぼすという欠点を有している。さらに、重合法によっ
て、ＳｉＯ２粒子を固定化する場合、材料選択性が非常
に狭くなるという欠点を有している。さらに表面に付着
している微粒子の量によりトナーそれぞれで帯電量が異
なり、画質に悪影響を与えるという欠点を有している。[Problems to be Solved by the Invention] However, in the above-mentioned adhesion method, the adhesion force of the fine particles adhering to the surface is weak;
It has the drawback that it peels off from the toner surface during toner transport and development, easily aggregates depending on the ambient temperature in which it is used, and the development characteristics of the toner deteriorate due to blocking and caking. Furthermore, the peeled off particles contaminate the inside of the apparatus, resulting in negative effects such as image deterioration and mechanical failure. Furthermore, when SiO2 particles are immobilized by a polymerization method, there is a drawback that material selectivity becomes extremely narrow. Furthermore, each toner has a different amount of charge depending on the amount of fine particles attached to its surface, which has a disadvantage in that it adversely affects image quality.
【０００６】従って本発明の目的は、上記課題を解決す
るもので
１）凝集防止（保存性）
２）高流動性
３）微粒子飛散の防止
４）安定な帯電性
５）簡単な製法
上記特性を有するトナーの製造方法を提供するものであ
る。Therefore, the purpose of the present invention is to solve the above-mentioned problems by: 1) Preventing agglomeration (storability) 2) High fluidity 3) Preventing fine particle scattering 4) Stable charging property 5) Simple manufacturing method The present invention provides a method for producing a toner having the following properties.
【０００７】[0007]
【課題を解決するための手段】本発明のトナー製造方法
は、乾式現像法に使用し、少なくとも結着樹脂と着色剤
よりなる内核粒子の外表面に無機物微粒子と樹脂微粒子
を用いて樹脂被覆層を形成したトナーにおいて、内核粒
子の外表面に粒径が０．１μｍ以下である無機物微粒子
と粒径が１μｍ以下である樹脂微粒子の混合粒子を湿式
で付着させ、次に前記樹脂微粒子を溶解させる溶剤で処
理する事により、無機物微粒子を含む樹脂被覆層を形成
することを特徴とする。[Means for Solving the Problems] The toner manufacturing method of the present invention is used in a dry development method, and uses inorganic fine particles and resin fine particles on the outer surface of inner core particles consisting of at least a binder resin and a colorant to form a resin coating layer. In the toner in which a mixture of inorganic particles with a particle size of 0.1 μm or less and resin particles with a particle size of 1 μm or less is wet-adhered to the outer surface of the inner core particles, the resin particles are then dissolved. It is characterized by forming a resin coating layer containing inorganic fine particles by treating with a solvent.
【０００８】[0008]
【実施例】図１に本発明のトナー製造方法のフローチャ
ートを示す。少なくとも結着樹脂１と着色剤２からなる
原料を用いて混練粉砕法、スプレードライ法、重合法等
によりトナー内核６を作製する。次に、トナー内核６に
樹脂微粒子３と無機物微粒子４を付着させる外添処理９
を行い樹脂及び無機物微粒子外添内核粒子７を作製する
。次に樹脂及び無機物微粒子外添内核粒子７に樹脂微粒
子３を溶解する溶剤５を接触させ被膜処理１０を行い、
無機物微粒子含有樹脂被膜トナー８を作製する。本発明
に用いる内核粒子は結着樹脂と少なくとも１種類以上の
トナー成分を含有する粒子を使用する。トナー成分とし
ては、着色剤、電荷制御剤、磁性粉、導電剤、離型剤、
分散剤などを必要に応じて選択するものである。トナー
内核は、粒径１〜４０μｍのものを使用することができ
る。形状は球形でも不定型でも構わない。DESCRIPTION OF THE PREFERRED EMBODIMENTS FIG. 1 shows a flowchart of the toner manufacturing method of the present invention. A toner inner core 6 is produced using a raw material consisting of at least a binder resin 1 and a colorant 2 by a kneading and pulverizing method, a spray drying method, a polymerizing method, or the like. Next, an external addition process 9 in which fine resin particles 3 and fine inorganic particles 4 are attached to the toner inner core 6
In this way, inner core particles 7 with resin and inorganic fine particles externally added are prepared. Next, a coating treatment 10 is performed by bringing a solvent 5 that dissolves the resin particles 3 into contact with the inner core particles 7 to which the resin and inorganic particles are externally added.
A resin-coated toner 8 containing inorganic fine particles is prepared. The core particles used in the present invention are particles containing a binder resin and at least one type of toner component. Toner components include colorant, charge control agent, magnetic powder, conductive agent, release agent,
Dispersants and the like are selected as necessary. The toner inner core can have a particle size of 1 to 40 μm. The shape may be spherical or irregular.
【０００９】内核粒子表面に無機物微粒子と樹脂微粒子
の混合粉体を付着させる湿式の方法としては、内核粒子
表面と樹脂微粒子表面のゼータ電位差による静電付着力
を利用したヘテロ凝集法、混合分散液のボールミル等で
のミリングによる湿式ミリング法、粉体インク内核粒子
をカップリング剤で処理してから樹脂微粒子と混合、付
着処理するカップリング剤法、樹脂溶液樹脂粒子分散系
における界面沈澱法等が適応可能である。ヘテロ凝集法
では、内核粒子と樹脂微粒子の粒径比は３以上が好まし
く、また内核粒子と樹脂微粒子のゼータ電位は正負逆極
性になるように組成を調整することが好ましい。湿式ミ
リング法では、内核粒子と樹脂微粒子の粒径比は５以上
が好ましい。カップリング剤法では、内核粒子と樹脂微
粒子の粒径比は３以上が好ましく、内核粒子にシラン、
チタン、クロム、アルミ、有機リン、過酸化シリル等の
カップリング剤を添加、もしく表面処理し、樹脂微粒子
にはカップリング剤の官能基と反応可能な官能基を有す
るように組成を調整する必要がある。界面沈澱法では、
樹脂微粒子と溶解性が異なる樹脂の溶液に樹脂微粒子を
分散し、内核粒子を分散して樹脂が不溶性の溶剤を添加
することによる沈澱現象を利用して、内核粒子表面に樹
脂微微子を付着させる。Wet methods for adhering a mixed powder of inorganic fine particles and resin fine particles to the surface of the inner core particles include a heteroaggregation method that utilizes electrostatic adhesion due to the zeta potential difference between the surface of the inner core particles and the surface of the resin fine particles, and a mixed dispersion method. Wet milling method using a ball mill, etc., coupling agent method in which powder ink inner core particles are treated with a coupling agent and then mixed with resin fine particles for adhesion treatment, interfacial precipitation method in resin solution resin particle dispersion system, etc. Adaptable. In the heteroaggregation method, the particle size ratio of the inner core particles and the fine resin particles is preferably 3 or more, and the composition is preferably adjusted so that the zeta potentials of the inner core particles and the fine resin particles have opposite polarities. In the wet milling method, the particle size ratio of the inner core particles to the resin fine particles is preferably 5 or more. In the coupling agent method, the particle size ratio of the inner core particles and resin fine particles is preferably 3 or more, and the inner core particles include silane,
A coupling agent such as titanium, chromium, aluminum, organic phosphorus, silyl peroxide, etc. is added or surface treated, and the composition is adjusted so that the resin fine particles have a functional group that can react with the functional group of the coupling agent. There is a need. In the interfacial precipitation method,
Resin particles are dispersed in a solution of a resin that has a different solubility from that of the resin particles, and the resin particles are attached to the surface of the inner core particles using the precipitation phenomenon caused by dispersing the inner core particles and adding a solvent in which the resin is insoluble. .
【００１０】次に溶剤処理をする方法としては噴霧乾燥
法、液浸法などがあるが接触時間を制御できるものであ
れば何でも良い。好ましくは粉体コーティング装置、例
えば、ディスパーコート（日清製粉）、コートマイザー
（フロイント産業）などを使用する。[0010] Next, methods for solvent treatment include spray drying, liquid immersion, and the like, but any method may be used as long as the contact time can be controlled. Preferably, a powder coating device, such as Dispercoat (Nissin Seifun) or Coatmizer (Freund Sangyo), is used.
【００１１】内核粒子の組成としては特に限定されるも
のではなく、一般的なものを使用することができる。例
えば、結着樹脂としてはポリスチレン及び共重合体、例
えば、水素添加スチレン樹脂、スチレン・イソブチレン
共重合体、ＡＢＳ樹脂、ＡＳＡ樹脂、ＡＳ樹脂，ＡＡＳ
樹脂、ＡＣＳ樹脂、ＡＥＳ樹脂、スチレン・Ｐクロロス
チレン共重合体、スチレン・プロピレン共重合体、スチ
レン・ブタジエン架橋ポリマー、スチレン・ブタジエン
・塩素化パラフィン共重合体、スチレン・アリル・アル
コール共重合体、スチレン・ブタジエンゴムエマルジョ
ン、スチレン・マレイン酸エステル共重合体、スチレン
・イソブチレン共重合体、スチレン・無水マレイン酸共
重合体、アクリレート系樹脂あるいはメタアクリレート
系樹脂及びその共重合体、スチレン・アクリル系樹脂及
びその共重合体、例えば、スチレン・アクリル共重合体
、スチレン・ジエチルアミノ・エチルメタアクリレート
共重合体、スチレン・ブタジエン・アクリル酸エステル
共重合体、スチレン・メチルメタアクリレート共重合体
、スチレン・ｎーブチルメタアクリレート共重合体、ス
チレン・ジエチルアミノ・エチルメタアクリレート共重
合体、スチレン・メチルメタアクリレート・ｎ−ブチル
アクリレート共重合体、スチレン・メチルメタアクリレ
ート・ブチルアクリレート・Ｎ−（エトキシメチル）ア
クリルアミド共重合体、スチレン・グリシジルメタアク
リレート共重合体、スチレン・ブタジエン・ジメチル・
アミノエチルメタアクリレート共重合体、スチレン・ア
クリル酸エステル・マレイン酸エステル共重合体、スチ
レン・メタアクリル酸メチル・アクリル酸２ーエチルヘ
キシル共重合体、スチレン・ｎ−ブチルアリレート・エ
チルグリコールメタアクリレート共重合体、スチレン・
ｎ−ブチルメタアクリレート・アクリル酸共重合体、ス
チレン・ｎ−ブチルメタアクリレート・無水マレイン酸
共重合体、スチレン・ブチルアクリレート・イソブチル
マレイン酸ハーフエステル・ジビニルベンゼン共重合体
、ポリエステル及びその共重合体、ポリエチレン及びそ
の共重合体、エポキシ樹脂、シリコーン樹脂、ポリプロ
ピレン及びその共重合体、フッソ樹脂、ポリアミド樹脂
、ポリビニルアルコール樹脂、ポリウレタン樹脂、ポリ
ビニルブチラール樹脂などを一種類あるいは、二種類以
上ブレンドしたものを使用する事ができる。また、樹脂
以外の物質としてワックス等も使用することができる。
例えば、キャンデリラワックス、カルナバワックス、ラ
イスワックス等の植物系天然ワックス、みつろう、ラノ
リン等の動物系天然ワックス、モンタンワックス、オゾ
ケライト等の鉱物系天然ワックス、パラフィンワックス
、マイクロクリスタリンワックス、ペトロラタム等の天
然石油系ワックス、ポリエチレンワックス、フィッシャ
ー・トロプシュワックス等の合成炭化水素ワックス、モ
ンタンワックス誘導体、パラフィンワックス誘導体等の
変性ワックス、硬化ひまし油、硬化ひまし油誘導体等の
水素化ワックス、合成ワックス等のワックス類、ステア
リン酸、パルミチン酸等の高級脂肪酸類、低分子量ポリ
エチレン、酸化ポリエチレン、ポリプロピレン等のポリ
オレフィン、エチレン・アクリル酸共重合体、エチレン
・アクリル酸エステル共重合体、エチレン・酢酸ビニル
共重合体等のオレフィン共重合体を一種あるいは二種以
上を用いる。[0011] The composition of the inner core particles is not particularly limited, and any commonly used composition can be used. For example, binder resins include polystyrene and copolymers, such as hydrogenated styrene resins, styrene-isobutylene copolymers, ABS resins, ASA resins, AS resins, and AAS resins.
Resin, ACS resin, AES resin, styrene/P-chlorostyrene copolymer, styrene/propylene copolymer, styrene/butadiene crosslinked polymer, styrene/butadiene/chlorinated paraffin copolymer, styrene/allyl/alcohol copolymer, Styrene/butadiene rubber emulsion, styrene/maleic acid ester copolymer, styrene/isobutylene copolymer, styrene/maleic anhydride copolymer, acrylate resin or methacrylate resin and its copolymer, styrene/acrylic resin and copolymers thereof, such as styrene/acrylic copolymer, styrene/diethylamino/ethyl methacrylate copolymer, styrene/butadiene/acrylate ester copolymer, styrene/methyl methacrylate copolymer, styrene/n- Butyl methacrylate copolymer, styrene/diethylamino/ethyl methacrylate copolymer, styrene/methyl methacrylate/n-butyl acrylate copolymer, styrene/methyl methacrylate/butyl acrylate/N-(ethoxymethyl)acrylamide copolymer Coalescence, styrene/glycidyl methacrylate copolymer, styrene/butadiene/dimethyl/
Aminoethyl methacrylate copolymer, styrene/acrylic acid ester/maleic ester copolymer, styrene/methyl methacrylate/2-ethylhexyl acrylate copolymer, styrene/n-butyl arylate/ethyl glycol methacrylate copolymer Combined, styrene
n-butyl methacrylate/acrylic acid copolymer, styrene/n-butyl methacrylate/maleic anhydride copolymer, styrene/butyl acrylate/isobutyl maleic acid half ester/divinylbenzene copolymer, polyester and its copolymer , polyethylene and its copolymers, epoxy resins, silicone resins, polypropylene and its copolymers, fluorocarbon resins, polyamide resins, polyvinyl alcohol resins, polyurethane resins, polyvinyl butyral resins, etc., or a blend of two or more of them. It can be used. Moreover, wax etc. can also be used as a substance other than resin. For example, plant-based natural waxes such as candelilla wax, carnauba wax, and rice wax, animal-based natural waxes such as beeswax and lanolin, mineral-based natural waxes such as montan wax and ozokerite, and natural natural waxes such as paraffin wax, microcrystalline wax, and petrolatum. Petroleum waxes, polyethylene waxes, synthetic hydrocarbon waxes such as Fischer-Tropsch waxes, modified waxes such as montan wax derivatives and paraffin wax derivatives, hydrogenated waxes such as hydrogenated castor oil and hydrogenated castor oil derivatives, waxes such as synthetic waxes, and stearin. acids, higher fatty acids such as palmitic acid, polyolefins such as low molecular weight polyethylene, polyethylene oxide, and polypropylene, olefin copolymers such as ethylene/acrylic acid copolymers, ethylene/acrylic acid ester copolymers, and ethylene/vinyl acetate copolymers. One kind or two or more kinds of polymers are used.
【００１２】着色剤としてはカーボンブラック、スピリ
ットブラック、ニグロシンなどの黒色染・顔料を使用す
る。カラー用としては、フタロシアニン、ローダミンＢ
レーキ、ソーラピュアイエロー８Ｇ、キナクリドン、ポ
リタングストリン酸、インダスレンブルー、スルホンア
ミド誘導体などの染料、または顔料を使用することがで
きる。さらに、分散剤として、金属石鹸、ポリエチレン
グリコールなど、帯電制御剤として、電子受容性の有機
錯体、塩素化ポリエステル、ニトロフニン酸、第４級ア
ンモニウム塩、ピリジニル塩などを添加することができ
る。この他に磁性用トナーとして磁性粉末、例えば、Ｆ
ｅ３Ｏ４、Ｆｅ２Ｏ３、Ｆｅ、Ｃｒ、Ｎｉなどを用いる
。[0012] As the coloring agent, a black dye/pigment such as carbon black, spirit black, nigrosine, etc. is used. For color use, phthalocyanine, rhodamine B
Dyes such as Lake, Solar Pure Yellow 8G, quinacridone, polytungstophosphoric acid, industhrene blue, sulfonamide derivatives, or pigments can be used. Further, dispersants such as metal soaps and polyethylene glycol can be added, and charge control agents such as electron-accepting organic complexes, chlorinated polyesters, nitrofnic acids, quaternary ammonium salts, and pyridinyl salts can be added. In addition, magnetic powder such as F
e3O4, Fe2O3, Fe, Cr, Ni, etc. are used.
【００１３】次に本発明に用いる無機物微粒子としては
、Ｓｉ０２、ＴｉＯ２、Ｚｎ０、Ａｌ２Ｏ３（α型、β
型）、ＴｉＯＮ、ＴｉＢａＯ３、ＭｇＯ、ＺｒＯ２、Ｃ
ａＣＯ３、ＮｉＯ、ＳｎＯ、クレー、タルク、ケイ砂、
雲母、ＳｉＮ、ＳｉＣ、Ｂａ２ＳＯ４、カーボンブラッ
ク等の微粒子を使用する事ができる。また、樹脂微粒子
としてはポリメチルメタアクリレート、ポリエチルメタ
アクリレート、ポリｎーブチルメタアクリレート、ポリ
エステル、（スチレンーブタジエン）コポリマー、（Ｐ
ＶＣ、ＰＶＡ、ＰＶＡｃ）コポリマー、ポリγーメチル
ーグルタメート、フッ素樹脂、フッ化ビニリデン樹脂、
ベンゾクアナミン樹脂、シリコーン樹脂、エポキシ樹脂
、ナイロン６６／６、ナイロン１１、ナイロン１２、ポ
リスチレン樹脂、架橋ポリスチレン樹脂、フェノール樹
脂、メラミン樹脂、ポリオレフィン樹脂、ポリエチレン
樹脂、セルロース等を使用する。Next, as the inorganic fine particles used in the present invention, Si02, TiO2, Zn0, Al2O3 (α type, β type
type), TiON, TiBaO3, MgO, ZrO2, C
aCO3, NiO, SnO, clay, talc, silica sand,
Fine particles of mica, SiN, SiC, Ba2SO4, carbon black, etc. can be used. In addition, resin fine particles include polymethyl methacrylate, polyethyl methacrylate, poly n-butyl methacrylate, polyester, (styrene-butadiene) copolymer, (P
VC, PVA, PVAc) copolymer, polyγ-methyl-glutamate, fluororesin, vinylidene fluoride resin,
Benzoquanamine resin, silicone resin, epoxy resin, nylon 66/6, nylon 11, nylon 12, polystyrene resin, crosslinked polystyrene resin, phenol resin, melamine resin, polyolefin resin, polyethylene resin, cellulose, etc. are used.
【００１４】内核粒子の表面に混合粉体を付着させた後
、樹脂微粒子を溶解処理する溶剤としては、内核粒子及
び樹脂微粒子の材質により決定される。このため水系、
有機溶剤系等のものを使用する事ができる。[0014] After the mixed powder is attached to the surface of the inner core particles, the solvent used to dissolve the fine resin particles is determined depending on the materials of the inner core particles and the fine resin particles. For this reason, water systems,
Organic solvents can be used.
【００１５】以上前記方法によって無機物微粒子を含む
樹脂被覆層を形成する事により、処理後の分級などの操
作を必要とせず、簡単に流動性及び保存性の優れたトナ
ーを製造することができる。[0015] By forming a resin coating layer containing inorganic fine particles by the method described above, a toner with excellent fluidity and storage stability can be easily produced without the need for operations such as classification after treatment.
【００１６】以下に本実施例をより詳細に説明する。This embodiment will be explained in more detail below.
【００１７】（実施例１）
＜内核粒子の作製＞
スチレン／メチルアクリレート ９０ｗｔ％
ポリプロピレン
６ｗｔ％帯電制御剤
２ｗｔ％カーボンブラッ
ク ２ｗｔ％
上記組成の原料を使用し、スクリュウ押出機で混練し、
冷却後粗粉砕する。次にジェット粉砕機で微粉砕し、分
級して５〜２０μｍの内核粒子を作製した。(Example 1) <Preparation of inner core particles> Styrene/methyl acrylate 90wt%
polypropylene
6wt% charge control agent
2wt% carbon black 2wt%
Using raw materials with the above composition, kneading them in a screw extruder,
After cooling, coarsely grind. Next, it was finely pulverized with a jet pulverizer and classified to produce inner core particles of 5 to 20 μm.
【００１８】＜無機物微粒子と樹脂微粒子の付着＞無機
物微粒子として粒径０．０２μｍのＳｉＯ２、樹脂微粒
子としてポリブチルメタアクリレート（ＰＢＭＡ）を用
いた。ＰＢＭＡの粒径は０．４μｍ、ガラス転移点８３
℃のものを使用した。前記内核粒子を、樹脂粒子
ＰＢＭＡ（５％分散）無機物微粒子
ＳｉＯ２ （３％分散）からなる、分
散水溶液１０００ｍｌに混合し、ボールミルでの湿式ミ
リング法による付着処理を行い、続いてスプレードライ
ヤーにより乾燥、樹脂粒子付着トナーを得た。<Attachment of fine inorganic particles and fine resin particles> SiO2 having a particle size of 0.02 μm was used as the fine inorganic particles, and polybutyl methacrylate (PBMA) was used as the fine resin particles. The particle size of PBMA is 0.4 μm, and the glass transition point is 83.
℃ was used. The inner core particles are formed into resin particles.
PBMA (5% dispersion) inorganic fine particles were mixed with 1000 ml of a dispersion aqueous solution consisting of SiO2 (3% dispersion), subjected to adhesion treatment by wet milling with a ball mill, and then dried with a spray dryer to obtain resin particle-adhered toner. .
【００１９】この時ＳｉＯ２量は、ＰＢＭＡ表面への被
覆率換算で約１５０％であった。得られた粉体粒子の過
剰な、付着に寄与していないＰＢＭＡは分級した際、除
去されていた。分級後の粒子を電子顕微鏡観察したとこ
ろ、ＰＢＭＡ粒子とＳｉＯ２微粒子が内核粒子の表面に
剥がれず、付着していることが明かとなった。At this time, the amount of SiO2 was approximately 150% in terms of coverage on the PBMA surface. Excess PBMA that did not contribute to the adhesion of the obtained powder particles was removed during classification. When the particles after classification were observed under an electron microscope, it was revealed that the PBMA particles and SiO2 fine particles were not peeled off but were attached to the surface of the inner core particles.
【００２０】＜溶剤処理＞上記方法で作製した微粒子付
着の内核粒子に対して溶剤処理を行った。溶剤としてア
セトンを用いた。この溶剤に粉体を１．０秒接触させ、
その後、乾燥温度６０℃で噴霧乾燥してアセトンを蒸発
させた。この溶剤処理により得られた粒子は粒子同士の
結着も無く、粒子それぞれが独立した状態の集合体であ
った。また、本実施例で作製した粒子を電子顕微鏡によ
り断面観察したところ、内核粒子の表面に、０．２〜０
．３μｍの樹脂被覆層が形成されていた。さらに、樹脂
層にＳｉＯ２が均一に分散され、被覆層表面にもＳｉＯ
２が露出しているのが確認された。さらに、本実施例で
作製したトナーの安息角を測定したところ３０°の高流
動性を示した。<Solvent Treatment> The inner core particles with fine particles attached thereto produced by the above method were subjected to a solvent treatment. Acetone was used as the solvent. The powder is brought into contact with this solvent for 1.0 seconds,
Thereafter, the acetone was evaporated by spray drying at a drying temperature of 60°C. The particles obtained by this solvent treatment had no binding between particles, and each particle was an aggregate in an independent state. In addition, when the cross section of the particles produced in this example was observed using an electron microscope, it was found that 0.2 to 0.0
．． A resin coating layer of 3 μm was formed. Furthermore, SiO2 is uniformly dispersed in the resin layer, and SiO2 is also distributed on the surface of the coating layer.
2 was confirmed to be exposed. Furthermore, when the angle of repose of the toner produced in this example was measured, it showed high fluidity of 30°.
【００２１】さらに、本実施例で作製したトナーを一成
分非接触型現像機とＯＰＣ感光体を有するレーザープリ
ンターに搭載して、画像形成を行ったところブロッキン
グやケーキングを起こす事なく、鮮明な画像を形成する
ことができ、さらに３万枚の耐久テストを行ったところ
初期と同様にブロッキングやケーキングを起こす事なく
鮮明な画像を得ることができた。さらに本実施例で作製
したトナーを容器に密閉し、３０℃ー８０％の環境下に
三ヶ月間保存して同様なテストを行ったが凝集などの特
性上の劣化はなく、鮮明な画像を得ることができた。Furthermore, when the toner produced in this example was loaded into a laser printer having a one-component non-contact developing machine and an OPC photoreceptor and image formation was performed, a clear image was obtained without causing blocking or caking. After further durability testing of 30,000 sheets, it was possible to obtain clear images without blocking or caking, just as in the initial stage. Furthermore, the toner produced in this example was sealed in a container and stored in an environment of 30°C - 80% for three months, and a similar test was performed, but there was no deterioration in characteristics such as aggregation, and clear images were obtained. I was able to get it.
【００２２】（比較例１）実施例１で作製した内核粒子
を無機物微粒子であるＳｉＯ２と樹脂微粒子であるＰＢ
ＭＡからなる被覆層を表面に形成させないでそのまま実
施例１で用いたレーザプリンターに搭載して画像形成を
行ったところ、トナーの流動性が悪く、さらに現像器内
で凝集を起こし、鮮明な画像を形成することができなか
った。(Comparative Example 1) The inner core particles produced in Example 1 were mixed with SiO2, which is an inorganic fine particle, and PB, which is a resin fine particle.
When the laser printer used in Example 1 was used to form an image without forming a coating layer made of MA on the surface, the toner had poor fluidity and agglomerated in the developing device, resulting in a clear image. could not be formed.
【００２３】（比較例２）実施例１で作製した内核粒子
に、実施例１の＜無機物微粒子と樹脂微粒子の付着＞と
同様の方法で無機物微粒子と樹脂微粒子を付着させ、溶
剤処理をしないままのトナーを作製した。このトナーを
実施例１で用いたレーザープリンターに搭載して画像形
成を行ったところ、トナーの流動性が悪く、さらに現像
器内で凝集を起こし、鮮明な画像を形成することができ
なかった。また付着物の剥がれが生じ、現像器内の汚染
が起こっていた。また、このトナーの安息角を測定した
ところ、４８゜で流動性が悪かった。(Comparative Example 2) Inorganic fine particles and resin fine particles were attached to the inner core particles produced in Example 1 in the same manner as <Adhesion of inorganic fine particles and resin fine particles> in Example 1, and the inner core particles were left without solvent treatment. A toner was prepared. When this toner was loaded into the laser printer used in Example 1 to form an image, the toner had poor fluidity and agglomerated in the developing device, making it impossible to form a clear image. In addition, deposits were peeled off, causing contamination inside the developing device. Further, when the angle of repose of this toner was measured, it was 48°, indicating poor fluidity.
【００２４】（実施例２）本実施例では内核粒子として
、ワックスを主成分とし、磁性粉と着色剤を有する粒子
を用いた。その他、実施例１と同様に行った。(Example 2) In this example, particles containing wax as a main component, magnetic powder, and a colorant were used as the inner core particles. In other respects, the same procedure as in Example 1 was carried out.
【００２５】＜内核粒子の作製＞
パラフィンワックス ３０
ｗｔ％カルナバワックス
３０ｗｔ％Ｆｅ３Ｏ４
３８ｗｔ％カーボンブラック
２ｗｔ％上記組成
の原料を使用し、バッチ式混練機で混練し、冷却後粗粉
砕する。次に、ジェット粉砕機で微粉砕後、分級して平
均粒径１０μｍ、分布５〜２５μｍの内核粒子を作製し
た。<Preparation of inner core particles> Paraffin wax 30
wt% carnauba wax
30wt%Fe3O4
38wt% carbon black
Using raw materials having the above composition of 2 wt %, they are kneaded in a batch type kneader, cooled, and then coarsely pulverized. Next, the mixture was finely pulverized using a jet pulverizer, and then classified to produce inner core particles with an average particle diameter of 10 μm and a distribution of 5 to 25 μm.
【００２６】＜無機物微粒子と樹脂微粒子の付着＞実施
例１と同様なＰＢＭＡとＳｉＯ２を使用し、また同様な
組成で処理を行った。得られた粒子は実施例１と同様な
状態であった。<Attachment of inorganic fine particles and resin fine particles> The same PBMA and SiO2 as in Example 1 were used and the same composition was used for treatment. The obtained particles were in the same state as in Example 1.
【００２７】＜溶剤処理＞溶剤としてはキシレンを用い
た。接触時間は１秒、乾燥温度は６０℃で噴霧乾燥した
。得られた粒子は実施例１と同様に粒子同士の結着も無
く、粒子それぞれが独立した状態の集合体であった。
また、安息角を測定したところ３２°の高流動性を示し
た。（内核粒子の安息角は４５°以上であった。）さら
に、得られたトナーを電子顕微鏡により断面観察したと
ころ、内核粒子の表面に０．２〜０．３μｍの樹脂被覆
層が形成されていた。<Solvent Treatment> Xylene was used as the solvent. Spray drying was carried out at a contact time of 1 second and a drying temperature of 60°C. As in Example 1, the obtained particles were an aggregate in which each particle was independent, with no binding between the particles. Furthermore, when the angle of repose was measured, it was found to be 32°, indicating high fluidity. (The angle of repose of the inner core particles was 45° or more.) Furthermore, when the obtained toner was cross-sectionally observed using an electron microscope, a resin coating layer of 0.2 to 0.3 μm was formed on the surface of the inner core particles. Ta.
【００２８】さらに、本実施例で作製したトナーを一成
分磁気ブラシ現像機とＯＰＣ感光体を有するレーザープ
リンターに搭載して画像を形成したところブロッキング
やケーキングを起こす事無く、さらに定着温度１２０℃
という低温で鮮明な画像を形成する事が出来た。さらに
３万枚の耐久テストを行ったところ初期と同様にブロッ
キングやケーキングを起こす事なく鮮明な画像を得るこ
とができた。さらに本実施例で作製したトナーを容器に
密閉し、３０℃ー８０％の環境下に三ヶ月間保存して同
様なテストを行ったが凝集などの特性上の劣化はなく、
鮮明な画像を得ることができた。Furthermore, when the toner prepared in this example was loaded into a laser printer having a one-component magnetic brush developer and an OPC photoreceptor to form an image, no blocking or caking occurred, and the fixing temperature was 120°C.
It was possible to form clear images at such low temperatures. Furthermore, when we conducted a durability test of 30,000 sheets, we were able to obtain clear images without any blocking or caking, just like in the early days. Furthermore, the toner produced in this example was sealed in a container and stored in an environment of 30°C - 80% for three months and a similar test was conducted, but there was no deterioration in characteristics such as aggregation.
I was able to get a clear image.
【００２９】（実施例３）実施例２と同様な内核粒子と
無機物微粒子ＳｉＯ２、樹脂微粒子ＰＢＭＡを用い、無
機物微粒子と樹脂微粒子の粒径を変化させてトナーを作
製した。 表１と表２に実験Ｎｏと粒径の関係を示す。
表１は樹脂微粒子として実施例１で用いたＰＢＭＡ：０
．４μｍを用い、ＳｉＯ２粒子の粒径を変えて作製した
ものである。表２は無機物微粒子として実施例１で用い
たＳｉＯ２：０．０２μｍを用い、樹脂微粒子の粒径を
変えて作製したものである。(Example 3) A toner was prepared using the same inner core particles, inorganic fine particles SiO2, and resin fine particles PBMA as in Example 2, and by changing the particle sizes of the inorganic fine particles and the resin fine particles. Tables 1 and 2 show the relationship between experiment number and particle size. Table 1 shows the PBMA used in Example 1 as resin fine particles: 0
．． 4 μm, and the particle size of the SiO2 particles was changed. In Table 2, SiO2 used in Example 1 (0.02 μm) was used as the inorganic fine particles, and the particle size of the resin fine particles was changed.
【００３０】[0030]
【表１】[Table 1]
【００３１】[0031]
【表２】[Table 2]
【００３２】＜無機物微粒子と樹脂微粒子の付着＞実験
Ｎｏ．１〜３では、ＰＢＭＡは分散量を５％とし、Ｓｉ
Ｏ２の分散量をＰＢＭＡ表面に対する被覆率１５０％に
なるような組成で分散水溶液を作成した。また、実験Ｎ
ｏ．４〜６では、ＳｉＯ２の分散量を２％とし、ＰＢＭ
Ａの分散量をＳｉＯ２がＰＢＭＡ表面に対し被覆率１５
０％になるような分散水溶液を作成した。このような分
散水溶液１０００ｍｌに内核粒子を混合し、６０℃にて
１０時間混合攪拌してカップリング反応による付着処理
を行い、続いてスプレードライヤーにより乾燥、樹脂粒
子付着トナーを得た。<Adhesion of inorganic particles and resin particles> Experiment No. 1 to 3, PBMA has a dispersion amount of 5% and Si
An aqueous dispersion solution was prepared with a composition such that the amount of O2 dispersed would give a coverage of 150% to the PBMA surface. Also, experiment N
o. 4 to 6, the dispersion amount of SiO2 was set to 2%, and the PBM
The amount of dispersion of A is determined by the coverage rate of SiO2 on the PBMA surface of 15.
An aqueous dispersion solution was prepared so that the concentration was 0%. The inner core particles were mixed with 1000 ml of such aqueous dispersion solution, mixed and stirred at 60° C. for 10 hours to perform an adhesion treatment by coupling reaction, and then dried with a spray dryer to obtain a toner with resin particles attached.
【００３３】＜溶剤処理＞このトナーを実施例２＜溶剤
処理＞と同様の処理を行った。但し、接触時間は粒径に
応じて変化させた。前記材料により作製したトナーの結
果を表３に示す。さらにこれらのトナーについて、実施
例２と同様に画像形成を行い、画像評価した。その結果
を表４に示す。<Solvent Treatment> This toner was subjected to the same treatment as in Example 2 <Solvent Treatment>. However, the contact time was changed depending on the particle size. Table 3 shows the results of toners produced using the above materials. Furthermore, images were formed using these toners in the same manner as in Example 2, and the images were evaluated. The results are shown in Table 4.
【００３４】[0034]
【表３】[Table 3]
【００３５】[0035]
【表４】[Table 4]
【００３６】’鮮明’の定義は地かぶりが無く、画像濃
度が１．５以上の画像である。The definition of 'clear' is an image with no background fog and an image density of 1.5 or more.
【００３７】本実施例より、無機物微粒子の粒径が０．
１μｍよりも大きい場合、樹脂微粒子の粒径が１．０μ
ｍより大きい場合にはいずれも流動性が悪化し、画像も
鮮明なものが得られない事が明かとなった。According to this example, the particle size of the inorganic fine particles is 0.
If it is larger than 1 μm, the particle size of the resin fine particles is 1.0 μm.
It has become clear that when it is larger than m, the fluidity deteriorates and clear images cannot be obtained.
【００３８】（実施例４）実施例１の内核粒子とＰＢＭ
ＡおよびＳｉＯ２微粒子を用い、ＳｉＯ２量を変化させ
て行った。ＳｉＯ２量は樹脂微粒子表面への被覆率換算
で行った。表５に分散量を示す。(Example 4) Inner core particles and PBM of Example 1
A and SiO2 fine particles were used and the amount of SiO2 was varied. The amount of SiO2 was determined by converting the coverage onto the surface of the resin particles. Table 5 shows the amount of dispersion.
【００３９】これらの分散比で、分散水溶液１０００ｍ
ｌを作成し、２４時間混合攪拌して、ヘテロ凝集法によ
り付着処理を行い、続いてスプレードライヤーにより乾
燥と乳化剤溶解被膜化を同時に行い樹脂被膜トナーを作
製した。With these dispersion ratios, 1000 m of the dispersion aqueous solution
1 was prepared, mixed and stirred for 24 hours, and an adhesion treatment was performed by a heterocoagulation method. Subsequently, drying and emulsifier-dissolving coating were simultaneously performed using a spray dryer to produce a resin-coated toner.
【００４０】さらに、実施例１の＜溶剤処理＞と同様に
処理を行ってそれぞれトナーを作製した。これらのトナ
ーを用いて実施例１と同様に画像形成を行い、画像評価
を行った。結果を表６に示す。[0040] Further, the same treatment as <solvent treatment> in Example 1 was carried out to prepare respective toners. Images were formed using these toners in the same manner as in Example 1, and the images were evaluated. The results are shown in Table 6.
【００４１】[0041]
【表５】[Table 5]
【００４２】[0042]
【表６】[Table 6]
【００４３】尚、Ｎｏ．１０はＳｉＯ２の剥離が激しく
生じ、装置汚染を生じた。また、安息角はＮｏ．７と１
０が４６°、Ｎｏ．８が３１゜、Ｎｏ．９が３２°であ
った。 この様に換算被覆率が１００％より小さいと
表面露出ＳｉＯ２が減り流動性が低下する。さらにまた
、２００％を越えるとＳｉＯ２が過剰になり、逆に流動
性が低下するものと考えられる。[0043] Furthermore, No. In No. 10, severe peeling of SiO2 occurred, resulting in equipment contamination. Also, the angle of repose is No. 7 and 1
0 is 46°, No. 8 is 31°, No. 9 was 32°. As described above, when the converted coverage is less than 100%, the surface exposed SiO2 decreases and the fluidity decreases. Furthermore, if it exceeds 200%, SiO2 becomes excessive, which is thought to conversely reduce fluidity.
【００４４】以上実施例を述べたが、本発明はこれらの
実施例に限定されるものではなく、さらに、被覆層内に
その他のトナー成分を添加する事も可能である。Although the embodiments have been described above, the present invention is not limited to these embodiments, and it is also possible to add other toner components into the coating layer.
【００４５】[0045]
【発明の効果】以上述べたように本発明のトナーの製造
方法によれば、乾式現像法に使用し、少なくとも結着樹
脂と着色剤よりなる内核粒子の外表面に無機物微粒子と
樹脂微粒子を用いて樹脂被覆層を形成したトナーにおい
て、内核粒子の外表面に粒径が０．１μｍ以下である無
機物微粒子と粒径が１μｍ以下である樹脂微粒子の混合
粒子を湿式で付着させ、次に前記樹脂微粒子を溶解させ
る溶剤で処理する事により、無機物微粒子を含む樹脂被
覆層を形成するため、無機物微粒子が安定して付着し、
流動性が高く、凝集が生じることがほとんどない。また
、装置内の汚染がほとんどない。さらにトナーの帯電量
の経時変化がなく安定なため、画質が常に鮮明であると
いう効果を有する。As described above, according to the toner manufacturing method of the present invention, inorganic fine particles and resin fine particles are used on the outer surface of the inner core particles consisting of at least a binder resin and a colorant. In the toner having a resin coating layer formed thereon, mixed particles of inorganic fine particles having a particle size of 0.1 μm or less and resin fine particles having a particle size of 1 μm or less are wet-adhered to the outer surface of the inner core particles. By treating with a solvent that dissolves fine particles, a resin coating layer containing fine inorganic particles is formed, so the fine inorganic particles adhere stably.
It has high fluidity and almost no agglomeration occurs. Additionally, there is almost no contamination within the device. Furthermore, since the toner charge amount does not change over time and is stable, the image quality is always clear.
【００４６】さらに本発明のトナー製造方法によれば、
内核粒子の組成、構造に関わらず、種種の樹脂成分と無
機物成分からなる被覆層を均一に、かつ簡単に膜厚制御
を行って上記特性を満足するトナーを簡単に作製できる
という、これまでの多層構造トナー作製方法に較べて多
大の効果を有する。従って、本発明のトナー製造方法は
優れた機能を有する多層構造トナーの低コスト化にさら
に大きく貢献する事が出来る。Furthermore, according to the toner manufacturing method of the present invention,
Regardless of the composition and structure of the inner core particles, the coating layer consisting of various resin components and inorganic components can be uniformly and easily controlled in thickness, making it possible to easily produce toners that satisfy the above characteristics. This method has many effects compared to multilayer toner manufacturing methods. Therefore, the toner manufacturing method of the present invention can make an even greater contribution to reducing the cost of multilayered toners having excellent functionality.
【００４７】さらに、本発明のトナー製造方法は、電子
写真、静電記録、静電印刷、磁気記録法などを用いた画
像形成装置、つまり複写機、プリンター、ファクシミリ
などに広く応用することができる。Furthermore, the toner manufacturing method of the present invention can be widely applied to image forming apparatuses using electrophotography, electrostatic recording, electrostatic printing, magnetic recording, etc., such as copying machines, printers, facsimile machines, etc. .
【図１】本発明のトナー製造方法のフローチャート。FIG. 1 is a flowchart of the toner manufacturing method of the present invention.
【図２】本発明のトナー製造方法により作成されたトナ
ーの構成図。FIG. 2 is a configuration diagram of a toner produced by the toner production method of the present invention.
１・・・結着樹脂
２・・・着色剤
３・・・樹脂微粒子
４・・・無機物微粒子
５・・・溶剤
６・・・トナー内核
７・・・樹脂及び無機物微粒子外添内核粒子８・・・無
機物含有樹脂被膜トナー
９・・・外添処理
１０・・・被膜処理
１１・・・樹脂被膜層1... Binder resin 2... Colorant 3... Resin fine particles 4... Inorganic fine particles 5... Solvent 6... Toner inner core 7... Resin and inorganic fine particles externally added inner core particles 8. ...Inorganic substance-containing resin film toner 9...External addition treatment 10...Film treatment 11...Resin film layer
Claims (1)
樹脂と着色剤よりなる内核粒子の外表面に、無機物微粒
子と樹脂微粒子を用いて樹脂被覆層を形成したトナーに
おいて、内核粒子の外表面に粒径が０．１μｍ以下であ
る無機物微粒子と粒径が１μｍ以下である樹脂微粒子の
混合粒子を湿式で付着させ、次に前記樹脂微粒子を溶解
させる溶剤で処理する事により、無機物微粒子を含む樹
脂被覆層を形成することを特徴とするトナーの製造方法
。Claim 1: In a toner used in a dry development method, in which a resin coating layer is formed using inorganic fine particles and resin fine particles on the outer surface of the inner core particle consisting of at least a binder resin and a colorant, the outer surface of the inner core particle is Mixed particles of inorganic particles with a particle size of 0.1 μm or less and resin particles with a particle size of 1 μm or less are wet-adhered to the surface of the substrate, and then treated with a solvent that dissolves the resin particles, thereby containing inorganic particles. A method for producing a toner, comprising forming a resin coating layer.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3102541A JPH04333055A (en) | 1991-05-08 | 1991-05-08 | Production of toner |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3102541A JPH04333055A (en) | 1991-05-08 | 1991-05-08 | Production of toner |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH04333055A true JPH04333055A (en) | 1992-11-20 |
Family
ID=14330122
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP3102541A Pending JPH04333055A (en) | 1991-05-08 | 1991-05-08 | Production of toner |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH04333055A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010085495A (en) * | 2008-09-29 | 2010-04-15 | Sharp Corp | Method for manufacturing toner, toner, developer, developing apparatus, and image forming apparatus |
-
1991
- 1991-05-08 JP JP3102541A patent/JPH04333055A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010085495A (en) * | 2008-09-29 | 2010-04-15 | Sharp Corp | Method for manufacturing toner, toner, developer, developing apparatus, and image forming apparatus |
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