JPH04194868A - Manufacture of electric charge controlling resin particle - Google Patents
Manufacture of electric charge controlling resin particleInfo
- Publication number
- JPH04194868A JPH04194868A JP2320196A JP32019690A JPH04194868A JP H04194868 A JPH04194868 A JP H04194868A JP 2320196 A JP2320196 A JP 2320196A JP 32019690 A JP32019690 A JP 32019690A JP H04194868 A JPH04194868 A JP H04194868A
- Authority
- JP
- Japan
- Prior art keywords
- particles
- toner
- monomers
- weight
- microparticles
- 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
- 239000002245 particle Substances 0.000 title claims abstract description 71
- 229920005989 resin Polymers 0.000 title claims abstract description 45
- 239000011347 resin Substances 0.000 title claims abstract description 45
- 238000004519 manufacturing process Methods 0.000 title claims description 9
- 239000007771 core particle Substances 0.000 claims abstract description 69
- 239000011859 microparticle Substances 0.000 claims abstract description 30
- 239000000725 suspension Substances 0.000 claims abstract description 25
- 239000000843 powder Substances 0.000 claims abstract description 17
- 238000010438 heat treatment Methods 0.000 claims abstract description 11
- 239000003381 stabilizer Substances 0.000 claims abstract description 11
- 238000010557 suspension polymerization reaction Methods 0.000 claims abstract description 8
- 229920000642 polymer Polymers 0.000 claims description 18
- 239000012736 aqueous medium Substances 0.000 claims description 15
- 239000000178 monomer Substances 0.000 abstract description 57
- 229920001577 copolymer Polymers 0.000 abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 14
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 abstract description 4
- 229920001519 homopolymer Polymers 0.000 abstract description 4
- AYJRCSIUFZENHW-DEQYMQKBSA-L barium(2+);oxomethanediolate Chemical compound [Ba+2].[O-][14C]([O-])=O AYJRCSIUFZENHW-DEQYMQKBSA-L 0.000 abstract description 3
- 125000004433 nitrogen atom Chemical group N* 0.000 abstract description 3
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 abstract description 2
- 239000008233 hard water Substances 0.000 abstract 2
- DPBJAVGHACCNRL-UHFFFAOYSA-N 2-(dimethylamino)ethyl prop-2-enoate Chemical compound CN(C)CCOC(=O)C=C DPBJAVGHACCNRL-UHFFFAOYSA-N 0.000 abstract 1
- UDWYGWMSVGVBCG-UHFFFAOYSA-N 2-(dimethylamino)prop-2-enoic acid Chemical compound CN(C)C(=C)C(O)=O UDWYGWMSVGVBCG-UHFFFAOYSA-N 0.000 abstract 1
- 229910006069 SO3H Inorganic materials 0.000 abstract 1
- 230000004927 fusion Effects 0.000 abstract 1
- 239000010419 fine particle Substances 0.000 description 21
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 18
- 238000006116 polymerization reaction Methods 0.000 description 16
- 239000003795 chemical substances by application Substances 0.000 description 13
- 230000015572 biosynthetic process Effects 0.000 description 12
- 239000003505 polymerization initiator Substances 0.000 description 12
- 238000003786 synthesis reaction Methods 0.000 description 12
- 239000000839 emulsion Substances 0.000 description 11
- 239000003995 emulsifying agent Substances 0.000 description 9
- -1 ethylene, Propylene Chemical group 0.000 description 8
- 238000000034 method Methods 0.000 description 8
- 238000003756 stirring Methods 0.000 description 8
- 125000000542 sulfonic acid group Chemical group 0.000 description 8
- CERQOIWHTDAKMF-UHFFFAOYSA-M Methacrylate Chemical compound CC(=C)C([O-])=O CERQOIWHTDAKMF-UHFFFAOYSA-M 0.000 description 7
- 229910052799 carbon Inorganic materials 0.000 description 7
- 238000009826 distribution Methods 0.000 description 7
- 239000004615 ingredient Substances 0.000 description 7
- 239000003999 initiator Substances 0.000 description 7
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
- JRKICGRDRMAZLK-UHFFFAOYSA-L persulfate group Chemical group S(=O)(=O)([O-])OOS(=O)(=O)[O-] JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 description 6
- 239000000049 pigment Substances 0.000 description 6
- 229910052708 sodium Inorganic materials 0.000 description 6
- 239000002904 solvent Substances 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 239000000975 dye Substances 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 108091008695 photoreceptors Proteins 0.000 description 5
- 239000011734 sodium Substances 0.000 description 5
- RCEJCSULJQNRQQ-UHFFFAOYSA-N 2-methylbutanenitrile Chemical compound CCC(C)C#N RCEJCSULJQNRQQ-UHFFFAOYSA-N 0.000 description 4
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 4
- 238000004140 cleaning Methods 0.000 description 4
- 239000003086 colorant Substances 0.000 description 4
- 239000006185 dispersion Substances 0.000 description 4
- 238000010556 emulsion polymerization method Methods 0.000 description 4
- 238000007720 emulsion polymerization reaction Methods 0.000 description 4
- 230000002209 hydrophobic effect Effects 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 150000003839 salts Chemical class 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 238000010558 suspension polymerization method Methods 0.000 description 4
- 229920002554 vinyl polymer Polymers 0.000 description 4
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 3
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical group [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 3
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 3
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 3
- 239000000654 additive Substances 0.000 description 3
- 229910000019 calcium carbonate Inorganic materials 0.000 description 3
- 238000013329 compounding Methods 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- SUPCQIBBMFXVTL-UHFFFAOYSA-N ethyl 2-methylprop-2-enoate Chemical compound CCOC(=O)C(C)=C SUPCQIBBMFXVTL-UHFFFAOYSA-N 0.000 description 3
- STVZJERGLQHEKB-UHFFFAOYSA-N ethylene glycol dimethacrylate Substances CC(=C)C(=O)OCCOC(=O)C(C)=C STVZJERGLQHEKB-UHFFFAOYSA-N 0.000 description 3
- 235000019333 sodium laurylsulphate Nutrition 0.000 description 3
- 229920003169 water-soluble polymer Polymers 0.000 description 3
- 239000011787 zinc oxide Substances 0.000 description 3
- 235000014692 zinc oxide Nutrition 0.000 description 3
- MYRTYDVEIRVNKP-UHFFFAOYSA-N 1,2-Divinylbenzene Chemical compound C=CC1=CC=CC=C1C=C MYRTYDVEIRVNKP-UHFFFAOYSA-N 0.000 description 2
- VXNZUUAINFGPBY-UHFFFAOYSA-N 1-Butene Chemical compound CCC=C VXNZUUAINFGPBY-UHFFFAOYSA-N 0.000 description 2
- AGBXYHCHUYARJY-UHFFFAOYSA-N 2-phenylethenesulfonic acid Chemical compound OS(=O)(=O)C=CC1=CC=CC=C1 AGBXYHCHUYARJY-UHFFFAOYSA-N 0.000 description 2
- QPQKUYVSJWQSDY-UHFFFAOYSA-N 4-phenyldiazenylaniline Chemical compound C1=CC(N)=CC=C1N=NC1=CC=CC=C1 QPQKUYVSJWQSDY-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
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- RRHGJUQNOFWUDK-UHFFFAOYSA-N Isoprene Chemical compound CC(=C)C=C RRHGJUQNOFWUDK-UHFFFAOYSA-N 0.000 description 2
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- QYKIQEUNHZKYBP-UHFFFAOYSA-N Vinyl ether Chemical compound C=COC=C QYKIQEUNHZKYBP-UHFFFAOYSA-N 0.000 description 2
- YKTSYUJCYHOUJP-UHFFFAOYSA-N [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] Chemical compound [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] YKTSYUJCYHOUJP-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 125000001931 aliphatic group Chemical group 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 2
- 239000003945 anionic surfactant Substances 0.000 description 2
- ADCOVFLJGNWWNZ-UHFFFAOYSA-N antimony trioxide Chemical compound O=[Sb]O[Sb]=O ADCOVFLJGNWWNZ-UHFFFAOYSA-N 0.000 description 2
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 2
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 description 2
- 239000001506 calcium phosphate Substances 0.000 description 2
- 239000003093 cationic surfactant Substances 0.000 description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 2
- 238000004132 cross linking Methods 0.000 description 2
- 235000014113 dietary fatty acids Nutrition 0.000 description 2
- 239000002612 dispersion medium Substances 0.000 description 2
- 238000012674 dispersion polymerization Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 239000000194 fatty acid Substances 0.000 description 2
- 229930195729 fatty acid Natural products 0.000 description 2
- 230000009477 glass transition Effects 0.000 description 2
- LRDFRRGEGBBSRN-UHFFFAOYSA-N isobutyronitrile Chemical compound CC(C)C#N LRDFRRGEGBBSRN-UHFFFAOYSA-N 0.000 description 2
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 description 2
- 239000001095 magnesium carbonate Substances 0.000 description 2
- 229910000021 magnesium carbonate Inorganic materials 0.000 description 2
- 239000006082 mold release agent Substances 0.000 description 2
- 150000005673 monoalkenes Chemical class 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000012299 nitrogen atmosphere Substances 0.000 description 2
- YWAKXRMUMFPDSH-UHFFFAOYSA-N pentene Chemical compound CCCC=C YWAKXRMUMFPDSH-UHFFFAOYSA-N 0.000 description 2
- 150000002978 peroxides Chemical class 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 2
- 239000010452 phosphate Substances 0.000 description 2
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 description 2
- JEXVQSWXXUJEMA-UHFFFAOYSA-N pyrazol-3-one Chemical compound O=C1C=CN=N1 JEXVQSWXXUJEMA-UHFFFAOYSA-N 0.000 description 2
- MNCGMVDMOKPCSQ-UHFFFAOYSA-M sodium;2-phenylethenesulfonate Chemical compound [Na+].[O-]S(=O)(=O)C=CC1=CC=CC=C1 MNCGMVDMOKPCSQ-UHFFFAOYSA-M 0.000 description 2
- 239000000454 talc Substances 0.000 description 2
- 229910052623 talc Inorganic materials 0.000 description 2
- 229920005992 thermoplastic resin Polymers 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 description 2
- 229920001567 vinyl ester resin Polymers 0.000 description 2
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 2
- 239000001993 wax Substances 0.000 description 2
- 229910000859 α-Fe Inorganic materials 0.000 description 2
- VWXLCWNPSOUPPE-UHFFFAOYSA-N (1-amino-2-methylpropylidene)azanium;chloride Chemical compound Cl.CC(C)C(N)=N VWXLCWNPSOUPPE-UHFFFAOYSA-N 0.000 description 1
- MFEVGQHCNVXMER-UHFFFAOYSA-L 1,3,2$l^{2}-dioxaplumbetan-4-one Chemical compound [Pb+2].[O-]C([O-])=O MFEVGQHCNVXMER-UHFFFAOYSA-L 0.000 description 1
- OCQDPIXQTSYZJL-UHFFFAOYSA-N 1,4-bis(butylamino)anthracene-9,10-dione Chemical compound O=C1C2=CC=CC=C2C(=O)C2=C1C(NCCCC)=CC=C2NCCCC OCQDPIXQTSYZJL-UHFFFAOYSA-N 0.000 description 1
- PAOHAQSLJSMLAT-UHFFFAOYSA-N 1-butylperoxybutane Chemical compound CCCCOOCCCC PAOHAQSLJSMLAT-UHFFFAOYSA-N 0.000 description 1
- XHAFIUUYXQFJEW-UHFFFAOYSA-N 1-chloroethenylbenzene Chemical compound ClC(=C)C1=CC=CC=C1 XHAFIUUYXQFJEW-UHFFFAOYSA-N 0.000 description 1
- UZKWTJUDCOPSNM-UHFFFAOYSA-N 1-ethenoxybutane Chemical compound CCCCOC=C UZKWTJUDCOPSNM-UHFFFAOYSA-N 0.000 description 1
- WHFHDVDXYKOSKI-UHFFFAOYSA-N 1-ethenyl-4-ethylbenzene Chemical compound CCC1=CC=C(C=C)C=C1 WHFHDVDXYKOSKI-UHFFFAOYSA-N 0.000 description 1
- BXALRZFQYDYTGH-UHFFFAOYSA-N 1-oxoprop-2-ene-1-sulfonic acid Chemical compound OS(=O)(=O)C(=O)C=C BXALRZFQYDYTGH-UHFFFAOYSA-N 0.000 description 1
- COXCGWKSEPPDAA-UHFFFAOYSA-N 2,4-dimethylpentanenitrile Chemical compound CC(C)CC(C)C#N COXCGWKSEPPDAA-UHFFFAOYSA-N 0.000 description 1
- QHVBLSNVXDSMEB-UHFFFAOYSA-N 2-(diethylamino)ethyl prop-2-enoate Chemical compound CCN(CC)CCOC(=O)C=C QHVBLSNVXDSMEB-UHFFFAOYSA-N 0.000 description 1
- GOXQRTZXKQZDDN-UHFFFAOYSA-N 2-Ethylhexyl acrylate Chemical compound CCCCC(CC)COC(=O)C=C GOXQRTZXKQZDDN-UHFFFAOYSA-N 0.000 description 1
- FWLHAQYOFMQTHQ-UHFFFAOYSA-N 2-N-[8-[[8-(4-aminoanilino)-10-phenylphenazin-10-ium-2-yl]amino]-10-phenylphenazin-10-ium-2-yl]-8-N,10-diphenylphenazin-10-ium-2,8-diamine hydroxy-oxido-dioxochromium Chemical compound O[Cr]([O-])(=O)=O.O[Cr]([O-])(=O)=O.O[Cr]([O-])(=O)=O.Nc1ccc(Nc2ccc3nc4ccc(Nc5ccc6nc7ccc(Nc8ccc9nc%10ccc(Nc%11ccccc%11)cc%10[n+](-c%10ccccc%10)c9c8)cc7[n+](-c7ccccc7)c6c5)cc4[n+](-c4ccccc4)c3c2)cc1 FWLHAQYOFMQTHQ-UHFFFAOYSA-N 0.000 description 1
- MFYSUUPKMDJYPF-UHFFFAOYSA-N 2-[(4-methyl-2-nitrophenyl)diazenyl]-3-oxo-n-phenylbutanamide Chemical compound C=1C=CC=CC=1NC(=O)C(C(=O)C)N=NC1=CC=C(C)C=C1[N+]([O-])=O MFYSUUPKMDJYPF-UHFFFAOYSA-N 0.000 description 1
- MCWMYICYUGCRDY-UHFFFAOYSA-N 2-[2-[2-(2-hydroxyethoxy)ethoxy]ethoxy]ethyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OCCOCCOCCOCCO MCWMYICYUGCRDY-UHFFFAOYSA-N 0.000 description 1
- MLMGJTAJUDSUKA-UHFFFAOYSA-N 2-ethenyl-1h-imidazole Chemical compound C=CC1=NC=CN1 MLMGJTAJUDSUKA-UHFFFAOYSA-N 0.000 description 1
- OMIGHNLMNHATMP-UHFFFAOYSA-N 2-hydroxyethyl prop-2-enoate Chemical compound OCCOC(=O)C=C OMIGHNLMNHATMP-UHFFFAOYSA-N 0.000 description 1
- XEEYSDHEOQHCDA-UHFFFAOYSA-N 2-methylprop-2-ene-1-sulfonic acid Chemical compound CC(=C)CS(O)(=O)=O XEEYSDHEOQHCDA-UHFFFAOYSA-N 0.000 description 1
- KGIGUEBEKRSTEW-UHFFFAOYSA-N 2-vinylpyridine Chemical compound C=CC1=CC=CC=N1 KGIGUEBEKRSTEW-UHFFFAOYSA-N 0.000 description 1
- FRIBMENBGGCKPD-UHFFFAOYSA-N 3-(2,3-dimethoxyphenyl)prop-2-enal Chemical compound COC1=CC=CC(C=CC=O)=C1OC FRIBMENBGGCKPD-UHFFFAOYSA-N 0.000 description 1
- DEOCLXYPCQMPDP-UHFFFAOYSA-N 3-(2-aminoethylamino)propyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OCCCNCCN DEOCLXYPCQMPDP-UHFFFAOYSA-N 0.000 description 1
- FGKYVGZYNGABJP-UHFFFAOYSA-N 3-(2-aminoethylamino)propyl prop-2-enoate Chemical compound NCCNCCCOC(=O)C=C FGKYVGZYNGABJP-UHFFFAOYSA-N 0.000 description 1
- XUYDVDHTTIQNMB-UHFFFAOYSA-N 3-(diethylamino)propyl prop-2-enoate Chemical compound CCN(CC)CCCOC(=O)C=C XUYDVDHTTIQNMB-UHFFFAOYSA-N 0.000 description 1
- UFQHFMGRRVQFNA-UHFFFAOYSA-N 3-(dimethylamino)propyl prop-2-enoate Chemical compound CN(C)CCCOC(=O)C=C UFQHFMGRRVQFNA-UHFFFAOYSA-N 0.000 description 1
- WUPHOULIZUERAE-UHFFFAOYSA-N 3-(oxolan-2-yl)propanoic acid Chemical compound OC(=O)CCC1CCCO1 WUPHOULIZUERAE-UHFFFAOYSA-N 0.000 description 1
- WOAMRAPSJUZQJV-UHFFFAOYSA-N 3-oxopent-4-ene-2-sulfonic acid Chemical compound OS(=O)(=O)C(C)C(=O)C=C WOAMRAPSJUZQJV-UHFFFAOYSA-N 0.000 description 1
- JCYPECIVGRXBMO-UHFFFAOYSA-N 4-(dimethylamino)azobenzene Chemical compound C1=CC(N(C)C)=CC=C1N=NC1=CC=CC=C1 JCYPECIVGRXBMO-UHFFFAOYSA-N 0.000 description 1
- NSWKKBKROCMOHA-UHFFFAOYSA-N 4-(naphthalen-1-yldiazenyl)naphthalen-1-ol Chemical compound Oc1ccc(N=Nc2cccc3ccccc23)c2ccccc12 NSWKKBKROCMOHA-UHFFFAOYSA-N 0.000 description 1
- DWDURZSYQTXVIN-UHFFFAOYSA-N 4-[(4-aminophenyl)-(4-methyliminocyclohexa-2,5-dien-1-ylidene)methyl]aniline Chemical compound C1=CC(=NC)C=CC1=C(C=1C=CC(N)=CC=1)C1=CC=C(N)C=C1 DWDURZSYQTXVIN-UHFFFAOYSA-N 0.000 description 1
- DBCAQXHNJOFNGC-UHFFFAOYSA-N 4-bromo-1,1,1-trifluorobutane Chemical compound FC(F)(F)CCCBr DBCAQXHNJOFNGC-UHFFFAOYSA-N 0.000 description 1
- WSSSPWUEQFSQQG-UHFFFAOYSA-N 4-methyl-1-pentene Chemical compound CC(C)CC=C WSSSPWUEQFSQQG-UHFFFAOYSA-N 0.000 description 1
- SOJMSFGCUDLHBZ-UHFFFAOYSA-N 4-methyl-3-oxopent-4-ene-2-sulfonic acid Chemical compound OS(=O)(=O)C(C)C(=O)C(C)=C SOJMSFGCUDLHBZ-UHFFFAOYSA-N 0.000 description 1
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 description 1
- RGCKGOZRHPZPFP-UHFFFAOYSA-N Alizarin Natural products C1=CC=C2C(=O)C3=C(O)C(O)=CC=C3C(=O)C2=C1 RGCKGOZRHPZPFP-UHFFFAOYSA-N 0.000 description 1
- 239000005995 Aluminium silicate Substances 0.000 description 1
- RMMXTBMQSGEXHJ-UHFFFAOYSA-N Aminophenazone Chemical compound O=C1C(N(C)C)=C(C)N(C)N1C1=CC=CC=C1 RMMXTBMQSGEXHJ-UHFFFAOYSA-N 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- 239000004908 Emulsion polymer Substances 0.000 description 1
- JIGUQPWFLRLWPJ-UHFFFAOYSA-N Ethyl acrylate Chemical compound CCOC(=O)C=C JIGUQPWFLRLWPJ-UHFFFAOYSA-N 0.000 description 1
- 239000004606 Fillers/Extenders Substances 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- 229910002321 LaFeO3 Inorganic materials 0.000 description 1
- YIVJZNGAASQVEM-UHFFFAOYSA-N Lauroyl peroxide Chemical compound CCCCCCCCCCCC(=O)OOC(=O)CCCCCCCCCCC YIVJZNGAASQVEM-UHFFFAOYSA-N 0.000 description 1
- 229910000003 Lead carbonate Inorganic materials 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 description 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 description 1
- 229920002125 Sokalan® Polymers 0.000 description 1
- 241000519995 Stachys sylvatica Species 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 description 1
- 229910001308 Zinc ferrite Inorganic materials 0.000 description 1
- 239000005083 Zinc sulfide Substances 0.000 description 1
- JHNCXGXWSIOXSX-UHFFFAOYSA-N [Nd+3].[O-2].[Fe+2] Chemical compound [Nd+3].[O-2].[Fe+2] JHNCXGXWSIOXSX-UHFFFAOYSA-N 0.000 description 1
- NEKNPTMOEUCRLW-UHFFFAOYSA-N [O-2].[Fe+2].[Gd+3] Chemical compound [O-2].[Fe+2].[Gd+3] NEKNPTMOEUCRLW-UHFFFAOYSA-N 0.000 description 1
- GZHZIMFFZGAOGY-UHFFFAOYSA-N [O-2].[Fe+2].[La+3] Chemical compound [O-2].[Fe+2].[La+3] GZHZIMFFZGAOGY-UHFFFAOYSA-N 0.000 description 1
- WQHONKDTTOGZPR-UHFFFAOYSA-N [O-2].[O-2].[Mn+2].[Fe+2] Chemical compound [O-2].[O-2].[Mn+2].[Fe+2] WQHONKDTTOGZPR-UHFFFAOYSA-N 0.000 description 1
- AUNAPVYQLLNFOI-UHFFFAOYSA-L [Pb++].[Pb++].[Pb++].[O-]S([O-])(=O)=O.[O-][Cr]([O-])(=O)=O.[O-][Mo]([O-])(=O)=O Chemical compound [Pb++].[Pb++].[Pb++].[O-]S([O-])(=O)=O.[O-][Cr]([O-])(=O)=O.[O-][Mo]([O-])(=O)=O AUNAPVYQLLNFOI-UHFFFAOYSA-L 0.000 description 1
- 239000003082 abrasive agent Substances 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 150000007824 aliphatic compounds Chemical class 0.000 description 1
- HFVAFDPGUJEFBQ-UHFFFAOYSA-M alizarin red S Chemical compound [Na+].O=C1C2=CC=CC=C2C(=O)C2=C1C=C(S([O-])(=O)=O)C(O)=C2O HFVAFDPGUJEFBQ-UHFFFAOYSA-M 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 150000003973 alkyl amines Chemical class 0.000 description 1
- 150000008055 alkyl aryl sulfonates Chemical class 0.000 description 1
- XYLMUPLGERFSHI-UHFFFAOYSA-N alpha-Methylstyrene Chemical compound CC(=C)C1=CC=CC=C1 XYLMUPLGERFSHI-UHFFFAOYSA-N 0.000 description 1
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
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- 235000012211 aluminium silicate Nutrition 0.000 description 1
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- GHPGOEFPKIHBNM-UHFFFAOYSA-N antimony(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Sb+3].[Sb+3] GHPGOEFPKIHBNM-UHFFFAOYSA-N 0.000 description 1
- IRERQBUNZFJFGC-UHFFFAOYSA-L azure blue Chemical compound [Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[S-]S[S-].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-] IRERQBUNZFJFGC-UHFFFAOYSA-L 0.000 description 1
- QFFVPLLCYGOFPU-UHFFFAOYSA-N barium chromate Chemical compound [Ba+2].[O-][Cr]([O-])(=O)=O QFFVPLLCYGOFPU-UHFFFAOYSA-N 0.000 description 1
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 1
- 229910002113 barium titanate Inorganic materials 0.000 description 1
- RTVHKGIVFVKLDJ-UHFFFAOYSA-N barium(2+);iron(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[Fe+3].[Fe+3].[Ba+2] RTVHKGIVFVKLDJ-UHFFFAOYSA-N 0.000 description 1
- 239000000981 basic dye Substances 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 239000003738 black carbon Substances 0.000 description 1
- BOOMOFPAGCSKKE-UHFFFAOYSA-N butane-2-sulfonic acid;prop-2-enamide Chemical compound NC(=O)C=C.CCC(C)S(O)(=O)=O BOOMOFPAGCSKKE-UHFFFAOYSA-N 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
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- HTUDBOWEKWIOCZ-UHFFFAOYSA-N cadmium(2+) mercury(1+) sulfide Chemical compound [S-2].[Cd+2].[Hg+] HTUDBOWEKWIOCZ-UHFFFAOYSA-N 0.000 description 1
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- 229910052791 calcium Inorganic materials 0.000 description 1
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- 229910000389 calcium phosphate Inorganic materials 0.000 description 1
- 235000011010 calcium phosphates Nutrition 0.000 description 1
- AOWKSNWVBZGMTJ-UHFFFAOYSA-N calcium titanate Chemical compound [Ca+2].[O-][Ti]([O-])=O AOWKSNWVBZGMTJ-UHFFFAOYSA-N 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- JBTHDAVBDKKSRW-UHFFFAOYSA-N chembl1552233 Chemical compound CC1=CC(C)=CC=C1N=NC1=C(O)C=CC2=CC=CC=C12 JBTHDAVBDKKSRW-UHFFFAOYSA-N 0.000 description 1
- HBHZKFOUIUMKHV-UHFFFAOYSA-N chembl1982121 Chemical compound OC1=CC=C2C=CC=CC2=C1N=NC1=CC=C([N+]([O-])=O)C=C1[N+]([O-])=O HBHZKFOUIUMKHV-UHFFFAOYSA-N 0.000 description 1
- YOCIQNIEQYCORH-UHFFFAOYSA-M chembl2028361 Chemical compound [Na+].OC1=CC=C2C=C(S([O-])(=O)=O)C=CC2=C1N=NC1=CC=CC=C1 YOCIQNIEQYCORH-UHFFFAOYSA-M 0.000 description 1
- 229910000423 chromium oxide Inorganic materials 0.000 description 1
- VQWFNAGFNGABOH-UHFFFAOYSA-K chromium(iii) hydroxide Chemical compound [OH-].[OH-].[OH-].[Cr+3] VQWFNAGFNGABOH-UHFFFAOYSA-K 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 239000011362 coarse particle Substances 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- 229910021446 cobalt carbonate Inorganic materials 0.000 description 1
- ZOTKGJBKKKVBJZ-UHFFFAOYSA-L cobalt(2+);carbonate Chemical compound [Co+2].[O-]C([O-])=O ZOTKGJBKKKVBJZ-UHFFFAOYSA-L 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- XCJYREBRNVKWGJ-UHFFFAOYSA-N copper(II) phthalocyanine Chemical compound [Cu+2].C12=CC=CC=C2C(N=C2[N-]C(C3=CC=CC=C32)=N2)=NC1=NC([C]1C=CC=CC1=1)=NC=1N=C1[C]3C=CC=CC3=C2[N-]1 XCJYREBRNVKWGJ-UHFFFAOYSA-N 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- OWMBTIRJFMGPAC-UHFFFAOYSA-N dimethylamino 2-methylprop-2-enoate Chemical compound CN(C)OC(=O)C(C)=C OWMBTIRJFMGPAC-UHFFFAOYSA-N 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
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- NHOGGUYTANYCGQ-UHFFFAOYSA-N ethenoxybenzene Chemical compound C=COC1=CC=CC=C1 NHOGGUYTANYCGQ-UHFFFAOYSA-N 0.000 description 1
- GFJVXXWOPWLRNU-UHFFFAOYSA-N ethenyl formate Chemical compound C=COC=O GFJVXXWOPWLRNU-UHFFFAOYSA-N 0.000 description 1
- UIWXSTHGICQLQT-UHFFFAOYSA-N ethenyl propanoate Chemical compound CCC(=O)OC=C UIWXSTHGICQLQT-UHFFFAOYSA-N 0.000 description 1
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 description 1
- FPVGTPBMTFTMRT-NSKUCRDLSA-L fast yellow Chemical compound [Na+].[Na+].C1=C(S([O-])(=O)=O)C(N)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 FPVGTPBMTFTMRT-NSKUCRDLSA-L 0.000 description 1
- 235000019233 fast yellow AB Nutrition 0.000 description 1
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- 238000001914 filtration Methods 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- HTENFZMEHKCNMD-UHFFFAOYSA-N helio brilliant orange rk Chemical compound C1=CC=C2C(=O)C(C=C3Br)=C4C5=C2C1=C(Br)C=C5C(=O)C1=CC=CC3=C14 HTENFZMEHKCNMD-UHFFFAOYSA-N 0.000 description 1
- MLRKYSNODSLPAB-UHFFFAOYSA-N hex-1-yn-1-ol Chemical compound CCCCC#CO MLRKYSNODSLPAB-UHFFFAOYSA-N 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- BDAGIHXWWSANSR-NJFSPNSNSA-N hydroxyformaldehyde Chemical compound O[14CH]=O BDAGIHXWWSANSR-NJFSPNSNSA-N 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 230000005865 ionizing radiation Effects 0.000 description 1
- 150000004698 iron complex Chemical class 0.000 description 1
- ADCBYGNHJOLWLB-UHFFFAOYSA-N iron(2+) oxygen(2-) yttrium(3+) Chemical compound [Y+3].[O-2].[Fe+2] ADCBYGNHJOLWLB-UHFFFAOYSA-N 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- YOBAEOGBNPPUQV-UHFFFAOYSA-N iron;trihydrate Chemical compound O.O.O.[Fe].[Fe] YOBAEOGBNPPUQV-UHFFFAOYSA-N 0.000 description 1
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 1
- 238000004898 kneading Methods 0.000 description 1
- 239000006233 lamp black Substances 0.000 description 1
- 239000004816 latex Substances 0.000 description 1
- 229920000126 latex Polymers 0.000 description 1
- PIJPYDMVFNTHIP-UHFFFAOYSA-L lead sulfate Chemical compound [PbH4+2].[O-]S([O-])(=O)=O PIJPYDMVFNTHIP-UHFFFAOYSA-L 0.000 description 1
- ZTERWYZERRBKHF-UHFFFAOYSA-N magnesium iron(2+) oxygen(2-) Chemical compound [Mg+2].[O-2].[Fe+2].[O-2] ZTERWYZERRBKHF-UHFFFAOYSA-N 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 229940107698 malachite green Drugs 0.000 description 1
- FDZZZRQASAIRJF-UHFFFAOYSA-M malachite green Chemical compound [Cl-].C1=CC(N(C)C)=CC=C1C(C=1C=CC=CC=1)=C1C=CC(=[N+](C)C)C=C1 FDZZZRQASAIRJF-UHFFFAOYSA-M 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002609 medium Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- VENDXQNWODZJGB-UHFFFAOYSA-N n-(4-amino-5-methoxy-2-methylphenyl)benzamide Chemical compound C1=C(N)C(OC)=CC(NC(=O)C=2C=CC=CC=2)=C1C VENDXQNWODZJGB-UHFFFAOYSA-N 0.000 description 1
- CTIQLGJVGNGFEW-UHFFFAOYSA-L naphthol yellow S Chemical compound [Na+].[Na+].C1=C(S([O-])(=O)=O)C=C2C([O-])=C([N+]([O-])=O)C=C([N+]([O-])=O)C2=C1 CTIQLGJVGNGFEW-UHFFFAOYSA-L 0.000 description 1
- NQNBVCBUOCNRFZ-UHFFFAOYSA-N nickel ferrite Chemical compound [Ni]=O.O=[Fe]O[Fe]=O NQNBVCBUOCNRFZ-UHFFFAOYSA-N 0.000 description 1
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000012188 paraffin wax Substances 0.000 description 1
- 235000012736 patent blue V Nutrition 0.000 description 1
- PNJWIWWMYCMZRO-UHFFFAOYSA-N pent‐4‐en‐2‐one Natural products CC(=O)CC=C PNJWIWWMYCMZRO-UHFFFAOYSA-N 0.000 description 1
- WRAQQYDMVSCOTE-UHFFFAOYSA-N phenyl prop-2-enoate Chemical compound C=CC(=O)OC1=CC=CC=C1 WRAQQYDMVSCOTE-UHFFFAOYSA-N 0.000 description 1
- 239000004584 polyacrylic acid Substances 0.000 description 1
- 229920000767 polyaniline Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- 229920000098 polyolefin Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- HJWLCRVIBGQPNF-UHFFFAOYSA-N prop-2-enylbenzene Chemical compound C=CCC1=CC=CC=C1 HJWLCRVIBGQPNF-UHFFFAOYSA-N 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 235000012752 quinoline yellow Nutrition 0.000 description 1
- 239000004172 quinoline yellow Substances 0.000 description 1
- 229940051201 quinoline yellow Drugs 0.000 description 1
- IZMJMCDDWKSTTK-UHFFFAOYSA-N quinoline yellow Chemical compound C1=CC=CC2=NC(C3C(C4=CC=CC=C4C3=O)=O)=CC=C21 IZMJMCDDWKSTTK-UHFFFAOYSA-N 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 239000005871 repellent Substances 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
- 229910052711 selenium Inorganic materials 0.000 description 1
- 239000011669 selenium Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 125000004436 sodium atom Chemical group 0.000 description 1
- LJFWQNJLLOFIJK-UHFFFAOYSA-N solvent violet 13 Chemical compound C1=CC(C)=CC=C1NC1=CC=C(O)C2=C1C(=O)C1=CC=CC=C1C2=O LJFWQNJLLOFIJK-UHFFFAOYSA-N 0.000 description 1
- 239000012798 spherical particle Substances 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 229910000018 strontium carbonate Inorganic materials 0.000 description 1
- VEALVRVVWBQVSL-UHFFFAOYSA-N strontium titanate Chemical compound [Sr+2].[O-][Ti]([O-])=O VEALVRVVWBQVSL-UHFFFAOYSA-N 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- CVNKFOIOZXAFBO-UHFFFAOYSA-J tin(4+);tetrahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[Sn+4] CVNKFOIOZXAFBO-UHFFFAOYSA-J 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 229910000391 tricalcium phosphate Inorganic materials 0.000 description 1
- 235000019731 tricalcium phosphate Nutrition 0.000 description 1
- 229940078499 tricalcium phosphate Drugs 0.000 description 1
- RBKBGHZMNFTKRE-UHFFFAOYSA-K trisodium 2-[(2-oxido-3-sulfo-6-sulfonatonaphthalen-1-yl)diazenyl]benzoate Chemical compound C1=CC=C(C(=C1)C(=O)[O-])N=NC2=C3C=CC(=CC3=CC(=C2[O-])S(=O)(=O)O)S(=O)(=O)[O-].[Na+].[Na+].[Na+] RBKBGHZMNFTKRE-UHFFFAOYSA-K 0.000 description 1
- 235000013799 ultramarine blue Nutrition 0.000 description 1
- NLVXSWCKKBEXTG-UHFFFAOYSA-N vinylsulfonic acid Chemical compound OS(=O)(=O)C=C NLVXSWCKKBEXTG-UHFFFAOYSA-N 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- UGZADUVQMDAIAO-UHFFFAOYSA-L zinc hydroxide Chemical compound [OH-].[OH-].[Zn+2] UGZADUVQMDAIAO-UHFFFAOYSA-L 0.000 description 1
- 229940007718 zinc hydroxide Drugs 0.000 description 1
- 229910021511 zinc hydroxide Inorganic materials 0.000 description 1
- 229910052984 zinc sulfide Inorganic materials 0.000 description 1
- NDKWCCLKSWNDBG-UHFFFAOYSA-N zinc;dioxido(dioxo)chromium Chemical compound [Zn+2].[O-][Cr]([O-])(=O)=O NDKWCCLKSWNDBG-UHFFFAOYSA-N 0.000 description 1
- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical compound [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 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、電荷制御用樹脂粒子の製造方法に関し、より
詳しくは電子写真用トナー等に利用する電荷制御用樹脂
粒子の製造方法に関する。DETAILED DESCRIPTION OF THE INVENTION <Industrial Application Field> The present invention relates to a method for producing charge control resin particles, and more particularly to a method for producing charge control resin particles used in electrophotographic toners and the like.
〈従来の技術〉
電子写真法、静電印刷法、静電記録法等において使用さ
れる現像方法は、帯電、露光により感光体上に形成され
た静電潜像をトナーで現像し、現像したトナー像を転写
紙等の支持体上に転写すると共に、加熱ローラまたは加
圧ローラによりトナー像を支持体に定着させ、静電潜像
を可視化するものである。そして、感光体上に残留する
トナーを除去するために、クリーニングプレート等のク
リーニング部材によって感光体上に残留するトナーを掻
き取っている。<Prior art> Development methods used in electrophotography, electrostatic printing, electrostatic recording, etc. develop an electrostatic latent image formed on a photoreceptor by charging and exposure with toner. The toner image is transferred onto a support such as a transfer paper, and the toner image is fixed on the support using a heating roller or a pressure roller to visualize the electrostatic latent image. In order to remove the toner remaining on the photoreceptor, the toner remaining on the photoreceptor is scraped off by a cleaning member such as a cleaning plate.
前記トナーはキャリアと混合して現像剤を構成する二成
分現像剤あるいはトナーのみによる一成分現像剤として
静電潜像の現像に用いられる。The toner is used for developing an electrostatic latent image as a two-component developer mixed with a carrier to form a developer, or as a one-component developer consisting only of toner.
そして、トナーを用いて、現像工程で原稿画像を忠実に
再現するためには、各トナー粒子の帯電量を均一にし、
未帯電粒子による静電潜像以外−＼のトナーの移行や過
剰帯電粒子による現像器内でのトナーの蓄積や、静電潜
像へのトナーの付着量の減少による画像濃度の低下を防
止する必要がある。In order to faithfully reproduce the original image in the development process using toner, the amount of charge on each toner particle must be made uniform.
Prevents the migration of toner other than the electrostatic latent image due to uncharged particles, toner accumulation in the developing device due to excessively charged particles, and a decrease in image density due to a decrease in the amount of toner adhering to the electrostatic latent image. There is a need.
従来のトナーは、一般に、定着用樹脂を電荷制御剤等の
添加剤と共に加熱溶融して混練し、冷却後、粉砕して分
級する二とによって製造されている。Conventional toners are generally manufactured by heating, melting, and kneading a fixing resin together with additives such as a charge control agent, cooling, and then crushing and classifying the resin.
しかしなから、このような粉砕法によって製造されるト
ナーでは、トナーの粒度分布か広く、比較的粒度の大き
な粒子か含まれるという欠点かある。また、トナーの摩
擦帯電特性を制御するために電荷制御剤か定着樹脂に添
加されているか、電荷制御剤は定着樹脂中ての分散性か
悪く、摩擦帯電性を支配する粒子表面に存在させるため
には、多量の電荷制御剤を添加する必要かあり、経済的
ではなかった。However, toner produced by such a pulverization method has a drawback that the toner particle size distribution is wide and contains particles with relatively large particle sizes. Also, whether a charge control agent is added to the fixing resin to control the triboelectric charging properties of the toner, or whether the charge control agent has poor dispersibility in the fixing resin and is present on the particle surface where it controls the triboelectric charging properties. However, it is necessary to add a large amount of charge control agent, which is not economical.
このような問題点を解消するために、以下のように種々
のトナーか提案されている。In order to solve these problems, various toners have been proposed as described below.
（１）特公昭５９−３８５８３号公報に記載のように、
重合によって形成した核体粒子をラテックス水溶液中に
混合分散させ、水溶性無機塩を添加するか、あるいはｐ
Ｈを変化させて、核体粒子表面に微小粒子を沈降させ被
覆層を形成したトナー。(1) As described in Japanese Patent Publication No. 59-38583,
The core particles formed by polymerization are mixed and dispersed in an aqueous latex solution, and a water-soluble inorganic salt is added or p
A toner in which fine particles are precipitated on the surface of core particles to form a coating layer by changing H.
（２）特開昭６２−２２６１６２２６１６２号公報うに
、着色熱可塑性樹脂粒子と、フローテスタによる流出開
始温度か前記樹脂粒子のそれよりも高い微小樹脂粒子と
を加熱処理する二とにより、着色熱可塑性樹脂粒子の表
面に微小樹脂粒子を付着させたトナー。(2) Japanese Unexamined Patent Application Publication No. 62-22616226162 By heat-treating colored thermoplastic resin particles and fine resin particles whose outflow start temperature is higher than that of the resin particles by a flow tester, colored thermoplastic resin particles are produced. A toner with minute resin particles attached to the surface of resin particles.
（３）特開昭６３−９３３４６号公報に記載のように、
懸濁重合して製造した低軟化点の樹脂粒子の表面に０゜
２〜１ ｕｍの高軟化点の粒子を水媒体中で付着させた
トナー。(3) As described in Japanese Patent Application Laid-open No. 63-93346,
A toner in which particles with a high softening point of 0°2 to 1 um are adhered to the surface of resin particles with a low softening point produced by suspension polymerization in an aqueous medium.
（４）特開昭６４−４４９５２号公報に記載のように、
界面重合粒子の表面に塩化ヒニリデンエマルノヨンを付
着させたトナー。(4) As described in Japanese Patent Application Laid-Open No. 64-44952,
A toner in which hnylidene chloride emulsion is adhered to the surface of interfacial polymer particles.
〈発明か解決しようとする課題〉
しかしなから、これらのトナーはいずれもコア粒子に対
する微小粒子の付着力か弱く、そのためたとえ熱処理を
行ったとしても、微小粒子か剥離しやすく、場合によっ
ては微小粒子かコア粒子に全く付着しない結果となって
いた。また、コア粒子に微小粒子を付着させる際に、コ
ア粒子同士か凝集して粗大粒径のトナーか部分的に生成
するおそれかあり、このような粗大トナーは正常な転写
を妨げ、複写画像に、いわゆる白抜けを生しさせる原因
となっていた。<Invention or problem to be solved> However, in all of these toners, the adhesion of the fine particles to the core particles is weak, so even if heat treatment is performed, the fine particles easily peel off, and in some cases, the fine particles may peel off. However, the result was that it did not adhere to the core particles at all. Furthermore, when fine particles are attached to core particles, there is a risk that the core particles will aggregate and partially produce toner with a coarse particle size, and such coarse toner will interfere with normal transfer and cause problems in the copied image. , which caused so-called white spots.
そこて、本出願人は、先に、樹脂のコア粒子と微小粒子
とにそれぞれ水系媒体中で互いに反対電荷に帯電する極
性を付与することにより、それらを水系媒体中にて付着
させ、その状態で熱処理することにより互いに熱融着さ
せる技術を開発した（特願昭６３−１３０８６３号）。Therefore, the present applicant first imparted polarity to the core particles and microparticles of the resin so that they were charged to opposite charges in an aqueous medium, so that they adhered to each other in an aqueous medium, and in that state. We developed a technology for thermally fusing them together by heat treating them (Japanese Patent Application No. 130863/1986).
しかしなから、コア粒子および微小粒子のうち少なくと
も一方（通常はコア粒子）を懸濁重合法で合成する場合
、媒体中に添加される懸濁安定剤として水溶性高分子（
例えばポリビニルアルコール、デンプン等）を用いると
、二の水溶性高分子か生成重合体内に取り込まれて、吸
湿性に冨んだものとなるため、電荷制御用樹脂粒子をト
ナーとして使用した場合には高温高湿下における帯電性
か悪くなるという欠点かある。一方、分散安定剤として
難水溶性の無機粉末（リン酸カルシウム、炭酸カルシウ
ム、炭酸マグネシウム、炭酸）＼リウム等）を用いた場
合には、上記のような問題はないものの、使用した難水
溶性無機粉末かコア粒子と微小粒子との間に介在して、
雨粒子かその電気な引力にて付着するのか妨害され、従
ってこの状態て熱処理しても両者か充分に融着せず、ト
ナーとして使用した場合には帯電性に劣ったものになる
という問題かあ、った。However, when at least one of core particles and microparticles (usually core particles) is synthesized by a suspension polymerization method, a water-soluble polymer (
For example, when polyvinyl alcohol, starch, etc.) are used, the second water-soluble polymer is incorporated into the resulting polymer, making it highly hygroscopic, so when charge control resin particles are used as a toner, The drawback is that the charging performance is poor under high temperature and high humidity conditions. On the other hand, when a poorly water-soluble inorganic powder (calcium phosphate, calcium carbonate, magnesium carbonate, lium carbonate, etc.) is used as a dispersion stabilizer, the above-mentioned problems do not occur, but the slightly water-soluble inorganic powder used or interposed between the core particle and the microparticle,
The problem is that either the rain particles or their electrical attraction interferes with the adhesion, and therefore, even if heat treatment is performed in this state, the two do not fuse together sufficiently, resulting in a toner with poor charging properties. , it was.
本発明の主たる目的は、コア粒子と微小粒子との付着か
強固で耐久性にすぐれた電荷制御用の帯電性樹脂粒子を
提供することである。The main object of the present invention is to provide chargeable resin particles for charge control, in which the adhesion between core particles and fine particles is strong and durable.
本発明の他の目的は、高温高温環境下でも帯電性にすぐ
れた電荷制御用樹脂粒子の製造方法を提供することであ
る。Another object of the present invention is to provide a method for producing charge control resin particles that have excellent chargeability even under high temperature environments.
く課題を解決するだめの手段および作用〉本発明の電荷
制御用樹脂粒子の製造方法は、少なくとも一方か懸濁重
合により合成され、水系媒体中において互いに反対の電
荷を有する樹脂のコア粒子と微小粒子とを熱処理してコ
ア粒子の表面に微小粒子を融着させるものであって、前
記懸濁重合を懸濁安定剤として難水溶性無機粉末を用い
て行ない、ついで生成重合体の懸濁液を、前記難水溶性
無機粉末を溶解させるｐＨ値に調節した後、前記熱処理
を行うことを特徴とする。Means and Effects for Solving the Problems> The method for producing resin particles for charge control of the present invention is characterized in that at least one of them is synthesized by suspension polymerization, and in an aqueous medium, a resin core particle and a microscopic resin particle having opposite charges are synthesized. The microparticles are fused to the surface of the core particle by heat treatment of the particles, and the suspension polymerization is carried out using a poorly water-soluble inorganic powder as a suspension stabilizer, and then a suspension of the resulting polymer is prepared. is adjusted to a pH value that dissolves the poorly water-soluble inorganic powder, and then the heat treatment is performed.
すなわち、本発明では、懸濁重合に際して懸濁安定剤と
して難水溶性無機粉末を使用しても、コア粒子と微小粒
子とを熱処理にて融着させる前に、あらかじめ懸濁液Ｏ
ｐＨ値を調節して、難水溶性無機粉末を溶解させている
ので、コア粒子と微小粒子との付着か難水溶性無機粉末
によって妨害されるのか防止されるので、コア粒子と微
小粒子との融着か強固なものになる。That is, in the present invention, even if a poorly water-soluble inorganic powder is used as a suspension stabilizer during suspension polymerization, the suspension O
Since the pH value is adjusted to dissolve the poorly water-soluble inorganic powder, the adhesion between the core particles and the microparticles is prevented, and the adhesion between the core particles and the microparticles is prevented. It becomes fused or strong.
以下、本発明の詳細な説明する。The present invention will be explained in detail below.
コア粒子
本発明におけるコア粒子は、水系媒体中で正電荷を育す
るものか好適に採用される。Core particles The core particles used in the present invention are preferably those that develop positive charges in an aqueous medium.
このようなコア粒子を構成する重合体としては、分子中
に窒素原子を存するモノマー等のように、水系媒体中で
正の電荷を有するモノマーの単独重合体およびこのモノ
マーと他のモノマーとの共重合体のいずれてもよいか、
トナーとして用いる場合は耐湿性および電荷割面の上で
共重合体であるのか好ましい。Polymers constituting such core particles include homopolymers of monomers that have a positive charge in an aqueous medium, such as monomers containing nitrogen atoms in their molecules, and copolymers of monomers with other monomers. Can be either a polymer or
When used as a toner, a copolymer is preferred in terms of moisture resistance and charge ratio.
分子中に窒素原子を有するモノマーとしては、例えばツ
メチルアミノアクリレート、ツメチルアミノエチルアク
リレート、ジエチルアミノエチルアクリレート、ジエチ
ルアミノプロビルアクリし一ト、Ｎ−アミノエチルアミ
ノプロピルアクリレート、ジメチルアミノメタクリレー
ト、ンメチルアミノエチルメタクリレート、ジエチルア
ミンエチルメタクリレ−１・、ンエチルアミノブロビル
メタクリレート、Ｎ−アミノエチルアミノプロピルメタ
クリレート、ビニルピリシン、２−ビニルイミダゾール
、２−ヒドロキン−３−アクリルオキシプロピルメチル
アンモニウムクロライド、アクリロニトリル等の含窒素
モノマーかあけられる。Examples of monomers having a nitrogen atom in the molecule include trimethylaminoacrylate, trimethylaminoethyl acrylate, diethylaminoethyl acrylate, diethylaminopropylacrylate, N-aminoethylaminopropyl acrylate, dimethylaminomethacrylate, and dimethylaminopropyl acrylate. Contains ethyl methacrylate, diethylamine ethyl methacrylate-1, ethylaminobrobyl methacrylate, N-aminoethylaminopropyl methacrylate, vinylpyridine, 2-vinylimidazole, 2-hydroquine-3-acryloxypropylmethylammonium chloride, acrylonitrile, etc. Drilled with nitrogen monomer.
かかる含窒素モノマーと共重合する他のモノで−として
は、種々のラノカル重合性のモノマーがあげられ、例え
はビニル芳香族モノマー、アクリル系モノマー、ビニル
エステル系モノマー、ヒ二ルエーテル系モノマー、ノオ
レフィン系モノマー、モノオレフィン系モノマー等かあ
げられる。Other monomers that copolymerize with such nitrogen-containing monomers include various lanocal polymerizable monomers, such as vinyl aromatic monomers, acrylic monomers, vinyl ester monomers, vinyl ether monomers, Examples include olefin monomers and monoolefin monomers.
ビニル芳香族モノマーとしては、例えはスチレン、α−
メチルスチレン、ビニルトルエン、α−クロロスチレン
、ｏ、ｍ、ｐ−タロロスチレン、ｐ−エチルスチレン、
ソヒニルヘンセンなとかあげられる。Examples of vinyl aromatic monomers include styrene, α-
Methylstyrene, vinyltoluene, α-chlorostyrene, o, m, p-talolostyrene, p-ethylstyrene,
I can give you something like Sohi Nil Hensen.
アクリル系モノマーとしては、例えはメチルアクリレー
ト、エチルアクリレート、ブチルアクリレート、２−エ
チルへキシルアクリレート、ノクロへキシルアクリレー
ト、フェニルアクリレート、メチルメタクリレート、エ
チルメタクリレート、ブチルメタクリレート、ヘキノル
メタクリレ−１・、２−エチルへキシルメタクリレート
、２−ヒドロキシエチルアクリレート、３−ヒドロキノ
プロピルアクリレート、４−ヒドロキンブチルアクリレ
ート、２−ヒドロキンエチルメタクリレート、エチレン
グリコールジメタクリレート、テトラエチレングリコー
ルンメタクリレート等があげられる。Examples of acrylic monomers include methyl acrylate, ethyl acrylate, butyl acrylate, 2-ethylhexyl acrylate, nocrohexyl acrylate, phenyl acrylate, methyl methacrylate, ethyl methacrylate, butyl methacrylate, and hexynol methacrylate-1, 2. Examples include -ethylhexyl methacrylate, 2-hydroxyethyl acrylate, 3-hydroquinopropyl acrylate, 4-hydroquine butyl acrylate, 2-hydroquine ethyl methacrylate, ethylene glycol dimethacrylate, and tetraethylene glycol methacrylate.
ビニルエステル系モノマーとしては、例えはギ酸ヒニル
、耐酸ビニル、プロピオン酸ビニル等があげられる。Examples of vinyl ester monomers include vinyl formate, acid-resistant vinyl, and vinyl propionate.
ビニルエーテル系モノマーとしては、例えばビニル−ｎ
−ブチルエーテル、ビニルフェニルエーテル、ビニルシ
クロヘキソルエーテル等があげられる。Examples of vinyl ether monomers include vinyl-n
-butyl ether, vinyl phenyl ether, vinyl cyclohexol ether, etc.
ノオレフィン系モノマーとしては、例えはブタノエン、
イソプレン、クロロブトン等かあげられる。Examples of olefinic monomers include butanoene,
Examples include isoprene and chlorobutone.
モノオレフィン系モノマーとしては、例えはエチレン、
プロピレン、イノブチレン、ブテン−１、ペンテン−１
，４−メチルペンテン−１なとがあげられる。Examples of monoolefin monomers include ethylene,
Propylene, inobutylene, butene-1, pentene-1
, 4-methylpentene-1.
これらのモノマーのうち、分子量分布の制御や水系媒体
中で正荷電を存するモノマーとの共重合性ならびに相溶
性のうえて、スチレン系、アクリル系のモノマーを使用
するのか好ましい。Among these monomers, styrene-based and acrylic-based monomers are preferably used in view of control of molecular weight distribution, copolymerizability and compatibility with positively charged monomers in an aqueous medium.
共重合体における前記正荷電を有するモノマーと、無電
荷のラジカル重合性モノマーとの割合は、前記正荷電を
存するモノマーを２０重量９６以下、とくに１０重量％
以下の割合であるのか耐湿性を付与するうえて好ましく
、正荷電を有するモノマーの割合かこれより大きいとき
は得られるコア粒子か耐湿性に劣ったものとなる。The ratio of the positively charged monomer and the uncharged radically polymerizable monomer in the copolymer is such that the positively charged monomer is 20% by weight or less, particularly 10% by weight.
The following proportions are preferable in terms of imparting moisture resistance; if the proportion of the positively charged monomer is greater than this, the resulting core particles will have poor moisture resistance.
重合は、懸濁重合法で行われる。懸濁重合法における分
散媒としては、水またはアルコール類か使用される。分
散媒は上記モノマーの総量１００重量部に対して、通常
５０〜１０００重量部の割合で使用される。Polymerization is carried out by suspension polymerization. Water or alcohols are used as the dispersion medium in the suspension polymerization method. The dispersion medium is generally used in an amount of 50 to 1000 parts by weight based on 100 parts by weight of the total amount of the monomers.
重合開始剤としては、例えはアブヒスイソブチロニトリ
ル、２．２−一アゾヒス（２−メチルブチロニトリル）
等のアゾ化合物、クメンヒドロペルオキシド、ｔ−プチ
ルヒトロベルオキント、ジクミルペルオキノド、シーｔ
−ブチルペルオキシド、過酸化へンゾイル、過酸化ラウ
ロイル等の過酸化物等の油溶性開始剤か使用される。こ
の他にγ−線、加速電子線のようなイオン化放射線や各
種増感剤と組合せてもよい。As a polymerization initiator, for example, Abhis isobutyronitrile, 2,2-1 azohis (2-methylbutyronitrile)
Azo compounds such as cumene hydroperoxide, t-butylhydroberoquinide, dicumylperoquinide, sheet t
- Oil-soluble initiators such as peroxides such as butyl peroxide, henzoyl peroxide, lauroyl peroxide, etc. are used. In addition, it may be combined with ionizing radiation such as γ-rays and accelerated electron beams, and various sensitizers.
また、他の添加剤としては、着色剤かあげられる。本発
明の電荷制御用樹脂粒子をトナーとじて用いる場合に使
用される着色剤としては、以下に例示の顔料や油溶性染
料かあげられる。In addition, other additives include colorants. Examples of the coloring agent used when the charge control resin particles of the present invention are used in combination with a toner include the following pigments and oil-soluble dyes.
黒色
カーボンフ゛ラック、アセチレンフ゛ラック、ランプブ
ラック、アニリンブラック
黄色
黄鉛、亜鉛黄、カドミウムイエロー、黄色酸化鉄、ミネ
ラルファストイエロー、ニノケルチタシイエロー、ネー
ブルスイエロー、ナフトールイエローＳ、ハンサイエロ
ー〇、ハシサイエロー１０６１ヘンジンンイエローＧ１
ベンジソンイエローＧＲ、キノリンイエローレーキ、パ
ーマネントイエローＮＧＯ，タートランンレーキ、Ｃ，
Ｉ ソルベント・イエロー ２、Ｃ，Ｉ ソルベン
ト・イエロー ＋４、Ｃ，Ｉ ソルベント・イエロー
橙色
赤口黄鉛、モリブデンオレンジ、パーマネントオレンジ
ＧＴＲ，ピラゾロンオしンン、ハルカンオしンノ、イン
ダンスレンブリリアントオレンジＲＫ、ヘンンノンオレ
ンシＧ、インク〉スレシブリリアントオレンンＧＫ、Ｃ
，Ｉ ソルベント・オレンジ ７
赤色
ヘンガラ、カドミウムヒソ１−１鉛丹、硫化水銀カドミ
ウム、パーマネントレット４Ｒ，リソールレソト、ピラ
ゾロンレット、ウォソチレグレノトカルノウム塩、レー
キレットＤ、ブリリアントカーミノ６Ｂ、エオシンレー
キ、ローダミンレーキＢ１アリザリンレーキ、ブリリア
ントカーミン３Ｂ、Ｃ，Ｔ、 ソルベント・レット
３、Ｃ，１ソルベント・レット ２４、ＣＩ、ソルベン
ト・レット ２７
紫色
マンガン紫、ファストバイオレットＢ、メチルバイオレ
ットレーキ、Ｃ１，ソルベント・バイオレット１３
青色
群青、コバルトブルー、アルカリブルーレーキ、ヒフト
リアブルーレーキ、フタロシアニンブルー、無金属フタ
ロノアニンブルー、フタロソアニンブル一部分塩素化物
、ファストスカイブルー、インダンスレンブル−ＢＣ，
Ｃ，Ｉ ソルベント・ブルー ７、Ｃ，Ｉ ソルベ
ント・ブルー ３５緑色
クロムクリーン、酸化クロム、ピグメントクリーンＢ、
マラカイトグリーンレーキ、コアナルイエローグリーン
Ｇ、Ｃ，Ｉ ソルベント・グリーン １５
茶色
ｃ、ｒ、 ソルベント・ブラウン ５白色
亜鉛華、酸化チタン、アンチモン白、硫化亜鉛体質顔料
ハライド粉、炭酸バリウム、クレー、ンリカ、ホワイト
カーホン、タルク、アルミナホワイｌ〜導電性顔料
導電性カーボンブランク、アルミニウム粉等の各種金属
粉
磁性材料顔料
四三酸化鉄（ＦｅＪ４） 、三二酸化鉄（γＦｅ２Ｏ，
，八酸化鉄亜鉛（ＺｎＦｅ２０４） 、酸化鉄イツトリ
ウム（’ｌ’３ＦｅｓＯ＋２）、酸化鉄カドミウム（Ｃ
ｄＦｅ２０４）、酸化鉄ガドリニウム（Ｇｄ＊Ｆｅ１Ｏ
＋２） 、酸化鉄鋼（ＣｕＦｅ、０４）、酸化鉄錯（Ｐ
ｂＦｅ１２０１８） 、酸化鉄ニッケル（ＮｉＦｅ２Ｏ
４）、酸化鉄ネオジウム（ＮｄＦｅＯ＊）、酸化鉄バリ
ウム（ＢａＦｅ１２０＋ｉ） 、酸化鉄マグネシウム（
八（ｇＦｅ２０４）、酸化鉄マンガン
（ＭｎＦｅ２０４） 、酸化鉄ランタン（ＬａＦｅＯ３
）、鉄粉、コバルト粉、ニッケル粉等
光導電性顔料
酸化亜鉛、セレン、硫化カドミウム、セレン化カドミウ
ム等
これらの着色剤は、１種または２種以上を混合して用い
られ、充分なトナー画像濃度か得られる量、例えば樹脂
１００重量部当たりｏ′、５〜３０重量部、とくに１〜
２０重量部で用いられる。Black carbon flake, acetylene flake, lamp black, aniline black yellow yellow lead, zinc yellow, cadmium yellow, yellow iron oxide, mineral fast yellow, Ninoker Chitashi yellow, Nabels yellow, naphthol yellow S, Hansa yellow 〇, Hashisa yellow 1061 Henjin Yellow G1
Benjison Yellow GR, Quinoline Yellow Lake, Permanent Yellow NGO, Tartran Lake, C,
I Solvent Yellow 2, C, I Solvent Yellow +4, C, I Solvent Yellow Orange Red Yellow Lead, Molybdenum Orange, Permanent Orange GTR, Pyrazolone Oshin, Harkan Oshinno, Indanthrene Brilliant Orange RK, Hennon Ore Nshi G, Ink〉Threaded Brilliant Orange GK, C
, I Solvent Orange 7 Red Hengara, Cadmium Hiso 1-1 Red, Mercury Cadmium Sulfide, Permanent Ret 4R, Lysole Lesotho, Pyrazolone Ret, Wosotile Grenote Carnoum Salt, Lakelet D, Brilliant Carmino 6B, Eosin Lake, Rhodamine Lake B1 Alizarin Lake, Brilliant Carmine 3B, C, T, Solvent Lett
3, C, 1 Solvent Let 24, CI, Solvent Let 27 Purple Manganese Purple, Fast Violet B, Methyl Violet Lake, C1, Solvent Violet 13 Ultramarine Blue, Cobalt Blue, Alkaline Blue Lake, Hyftria Blue Lake, Phthalocyanine Blue, metal-free phthalonoamine blue, phthalosoanimble partially chlorinated product, fast sky blue, indanthremblu-BC,
C, I Solvent Blue 7, C, I Solvent Blue 35 Green Chrome Clean, Chromium Oxide, Pigment Clean B,
Malachite Green Lake, Coanal Yellow Green G, C, I Solvent Green 15 Brown C, R, Solvent Brown 5 White Zinc White, Titanium Oxide, Antimony White, Zinc Sulfide Extender Pigment Halide Powder, Barium Carbonate, Clay, Nrica, White carphone, talc, alumina white - Conductive pigment Conductive carbon blank, various metal powders such as aluminum powder Magnetic materials Pigments Triiron tetroxide (FeJ4), iron sesquioxide (γFe2O,
, zinc octoxide (ZnFe204), yttrium iron oxide ('l'3FesO+2), cadmium iron oxide (C
dFe204), iron gadolinium oxide (Gd*Fe1O
+2), steel oxide (CuFe, 04), iron complex oxide (P
bFe12018), iron nickel oxide (NiFe2O
4), neodymium iron oxide (NdFeO*), barium iron oxide (BaFe120+i), magnesium iron oxide (
8 (gFe204), iron manganese oxide (MnFe204), lanthanum iron oxide (LaFeO3)
), photoconductive pigments such as iron powder, cobalt powder, nickel powder, etc. zinc oxide, selenium, cadmium sulfide, cadmium selenide, etc. These colorants are used singly or in combination of two or more to produce a sufficient toner image. the concentration obtained, e.g. o' per 100 parts by weight of resin, from 5 to 30 parts by weight, especially from 1 to
It is used in an amount of 20 parts by weight.
また、所望によりそれ自体公知のトナー配合剤を添加す
ることもてきる。このようなトナー配合剤としては、例
えば脂肪族系樹脂、脂肪族金属塩類、高級脂肪酸類、脂
肪酸エステル類、その部分ケン化物類などの公知の脂肪
族系化合物からなる離型剤（オフセット防止剤）をあげ
る二とかでき、とくに低分子量（重量平均分子量か１０
００〜１００００）の脂肪族系樹脂か好適であり、具体
的には低分子量ポリプロピレン、低分子量ポリエチレン
、パラフィンワックス、炭素原子数４以上のすレフイン
単位からなる低分子量オレフィン重合体等の１種または
２種以上の組合せか適当てあり、他にンリコーンオイル
、各種ワックスも使用することかできる。これらのワッ
クスは一般に樹脂成分１００重量部に対して１〜５重量
部、とくに１．５〜３重量部で使用するのか好ましい。Additionally, toner compounding agents known per se may be added if desired. Such toner compounding agents include mold release agents (offset inhibitors) made of known aliphatic compounds such as aliphatic resins, aliphatic metal salts, higher fatty acids, fatty acid esters, and partially saponified products thereof. ), especially low molecular weight (weight average molecular weight or 10
00 to 10,000) is suitable, and specifically, one type of low molecular weight polypropylene, low molecular weight polyethylene, paraffin wax, low molecular weight olefin polymer consisting of a carbon unit of 4 or more carbon atoms, etc. A combination of two or more types may be used, and lilycorn oil and various waxes may also be used. These waxes are generally preferably used in an amount of 1 to 5 parts by weight, particularly 1.5 to 3 parts by weight, based on 100 parts by weight of the resin component.
また、他のトナー配合剤としては、電荷制御剤かあげら
れ、目的とする電荷制御用樹脂粒子か正帯電性か負帯電
性かに応して正電荷制御剤（例えは塩基性染料、アミノ
ピリン等の塩基性窒素原子を存する有機化合物）または
負電荷制御剤（例えは含金属染料等）かコア粒子の重量
部成分の１００重量部に対して０．００１〜５重量部の
割合で配合される。In addition, other toner compounding agents include charge control agents, and depending on whether the desired charge control resin particles are positively chargeable or negatively chargeable, positive charge control agents (such as basic dyes, aminopyrine, etc.) may be used. etc.) or a negative charge control agent (for example, a metal-containing dye, etc.) is blended in an amount of 0.001 to 5 parts by weight per 100 parts by weight of the components by weight of the core particle. Ru.
また、懸濁重合に際しては、懸濁安定剤として離水性の
無機粉末を使用する。かかる無機粉末としては、例えば
硫酸カルシウム、炭酸バリウム、硫酸鉛、硫酸ニッケル
アンモニウム、炭酸カルシウム、炭酸マグネシウム、リ
ン酸力ルンウム、炭酸コバルト、炭酸ストロンチウム、
炭酸鉛、水酸化アルミニウム、水酸化クロム、水酸化亜
鉛、水酸化スズ等の無機粉末かあげられ、これらはｐＨ
調節により水系媒体（水、アルコール等）に溶解する性
質を有する。Furthermore, during suspension polymerization, a water-repellent inorganic powder is used as a suspension stabilizer. Examples of such inorganic powders include calcium sulfate, barium carbonate, lead sulfate, nickel ammonium sulfate, calcium carbonate, magnesium carbonate, phosphoric acid, cobalt carbonate, strontium carbonate,
Examples include inorganic powders such as lead carbonate, aluminum hydroxide, chromium hydroxide, zinc hydroxide, and tin hydroxide.
It has the property of being soluble in aqueous media (water, alcohol, etc.) when adjusted.
懸濁安定剤の使用量は、通常樹脂成分の１００重量部に
対して３〜２０重量部であるのか適当である。The amount of the suspension stabilizer used is generally 3 to 20 parts by weight per 100 parts by weight of the resin component.
懸濁重合法における造粒は、ホモミキサー、ホモジナイ
ザーなとの高速剪断攪拌機によって行われ、コア粒子を
目的に応した粒径に調整することかできる。コア粒子を
トナーとして使用する場合は、中心粒径か１〜１５μｍ
程度を有するように調整するのか好ましい。Granulation in the suspension polymerization method is carried out using a high-speed shear stirrer such as a homomixer or homogenizer, and the core particles can be adjusted to a particle size suitable for the purpose. When using core particles as toner, the center particle diameter is 1 to 15 μm.
It is preferable to adjust to a certain degree.
重合は通常、温度５０〜１００°Ｃて２〜１２時間程度
行われる。Polymerization is usually carried out at a temperature of 50 to 100°C for about 2 to 12 hours.
微小粒子
前記のように水系媒体中で正の電荷を有するコア粒子を
使用したとき、微小粒子としては、このコア粒子に対し
て電気的に付着しうるように、水系媒体中で負の電荷を
有するものを使用する。Microparticles When a core particle having a positive charge in an aqueous medium is used as described above, the microparticle has a negative charge in an aqueous medium so that it can be electrically attached to the core particle. Use what you have.
このような微小粒子としては、例えば分子中にスルホン
酸基−３Ｏ３１（（ただし、式中の水素原子はナトリウ
ム原子、カリウム原子、カリウム原子と置換されて塩を
形成していてもよい）を有するモノマーの単独重合体も
しくは他のモノマーとの共重合体あるいは水系媒体中で
負の電荷を重合体に付与する過硫酸塩を重合開始剤とし
て用いた重合体（もしくは共重合体）が使用可能である
。Examples of such microparticles include, for example, those having a sulfonic acid group -3O31 ((however, the hydrogen atom in the formula may be substituted with a sodium atom, a potassium atom, or a potassium atom to form a salt) in the molecule. Homopolymers of monomers or copolymers with other monomers, or polymers (or copolymers) using persulfates as polymerization initiators, which impart a negative charge to the polymer in an aqueous medium, can be used. be.
電荷制御用樹脂粒子をトナーとして使用する場合、耐湿
性および電荷制御の上がら、スルポン酸基を有するモノ
マーの単独重合体を使用するよりも、該モノマーと他の
モノマーとの共重合体を使用するのか好ましい。When using resin particles for charge control as a toner, from the viewpoint of moisture resistance and charge control, a copolymer of this monomer and another monomer is used rather than a homopolymer of a monomer having a sulfonic acid group. Or preferable.
スルホン酸基を有するモノマーとしては、例えばスチレ
ンスルホン酸、ビニルスルホン酸、アクリルアミドメチ
ルプロパンスルホン酸、アクリルスルホン酸、メタクリ
ルスルホン酸、アクリル−２−エチルスルホン酸、メタ
クリル−２−エチルスルホン酸等、さらにこれらのナト
リウム、カリウム、カルシウム等の塩類かあげられ、と
くに電荷制御性、反応性等からスチレンスルホン酸を使
用するのか好ましい。これらのスルホン酸基を有するモ
ノマーは、後述する乳化共重合体において、乳化重合体
粒子の粒度調整剤として、あるいは重合反応の促進剤と
して機能すると共に、負帯電性トナーの帯電性の向上に
も有効である。Examples of monomers having a sulfonic acid group include styrenesulfonic acid, vinylsulfonic acid, acrylamide methylpropanesulfonic acid, acrylsulfonic acid, methacrylsulfonic acid, acryl-2-ethylsulfonic acid, methacryl-2-ethylsulfonic acid, and the like. These salts such as sodium, potassium, and calcium may be used, and styrene sulfonic acid is particularly preferred from the viewpoint of charge control properties and reactivity. These sulfonic acid group-containing monomers function as particle size regulators for emulsion polymer particles or as promoters of polymerization reactions in the emulsion copolymers described below, and also serve to improve the chargeability of negatively chargeable toners. It is valid.
また、スルホン酸基を有するモノマーと共重合する他の
モノマーとしては、前記コア粒子において正の電荷を有
するモノマーと共重合する他のモノマーかいずれも使用
可能である。この場合、スルホン酸基を有するモノマー
の割合は、耐湿性の上から、モノマー総量に対して１０
重量％以下、とくに０．５〜５重量％であるのが好まし
い。Further, as the other monomer that copolymerizes with the monomer having a sulfonic acid group, any other monomer that copolymerizes with the monomer having a positive charge in the core particles can be used. In this case, the proportion of monomers having sulfonic acid groups is 10
It is preferably less than 0.5% by weight, particularly 0.5 to 5% by weight.
重合には、小粒径の微小粒子か容易に得られる屯て、乳
化重合法か好適に採用される。乳化重合法は、水中で水
溶性の開始剤を用いて、乳化剤の存在下てモノマーの重
合を行うものであるか、乳化剤か重合体内に残留してい
ると、その吸湿性のために帯電性に慝影響を与えるため
、乳化剤はできる限り除去する必要かある。For polymerization, emulsion polymerization is preferably employed since fine particles with a small particle size can be easily obtained. In the emulsion polymerization method, monomers are polymerized in water using a water-soluble initiator in the presence of an emulsifier, or if the emulsifier remains in the polymer, it may become electrostatically charged due to its hygroscopicity. It is necessary to remove as much emulsifier as possible because it affects the
従って、乳化重合に際しては、乳化剤を使用しない、い
わゆる無乳化剤乳化重合を行うのか好ましい。この重合
法は、■反応性乳化剤を用いたり、・２比較的親水性の
モノマーを過硫酸塩系開始剤により無乳化剤乳化重合し
たノフ、■水溶性ポリマー、オリゴマー（例えはポリヒ
ニルアルコール等）を乳化剤の代わりに用いたり、■分
解型乳化剤を用いたり、あるいは■架橋型乳化剤を用い
たりして重合を行うものである。これらの無乳化剤乳化
重合法のいずれもか本発明における微小粒子を製造する
上で採用可能であるか、前記スルホン酸基を有するモノ
マーと同様に重合体で負電荷を有する過硫酸塩系の重合
開始剤（例えは過硫酸カリウム等）を使用する無乳化剤
乳化重合法を採用するのか電荷制御のうえてとくに好ま
しい。過硫酸塩系の重合開始剤の添加量は、モノマーの
１００重量部に対して１〜５重量部であるのか適当であ
る。Therefore, in emulsion polymerization, it is preferable to perform so-called emulsifier-free emulsion polymerization without using an emulsifier. This polymerization method involves (1) using a reactive emulsifier, (2) polymerization of relatively hydrophilic monomers without an emulsifier using a persulfate initiator, and (2) water-soluble polymers, oligomers (such as polyhinyl alcohol, etc.). ) in place of the emulsifier, (1) using a decomposition type emulsifier, or (2) using a crosslinking type emulsifier. Either of these emulsifier-free emulsion polymerization methods can be employed to produce the microparticles of the present invention, or polymerization of a persulfate-based polymer having a negative charge in the same manner as the monomer having a sulfonic acid group is possible. It is particularly preferable to employ an emulsifier-free emulsion polymerization method using an initiator (for example, potassium persulfate, etc.) in view of charge control. The amount of the persulfate-based polymerization initiator added is suitably 1 to 5 parts by weight per 100 parts by weight of the monomer.
また、過硫酸塩系の開始剤はそれ自体で重合体に負電荷
を与えるため、スルホン酸基を有する千ツマ−のほか、
負電荷を有しない他のモノマーを使用しても微小粒子に
負電荷を付与することかできる。この場合、過硫酸塩系
開始剤の添加量は、１〜３重量部であるのか適当である
。In addition, since persulfate-based initiators themselves give a negative charge to the polymer, in addition to sulfonic acid group-containing initiators,
Other monomers that do not have a negative charge can also be used to impart a negative charge to the microparticles. In this case, the amount of persulfate-based initiator added is suitably 1 to 3 parts by weight.
また、乳化重合法に代えて、分散重合法を用いて微小粒
子を作成してもよい。ここで、分散重合法とは、モノマ
ーを着色剤、離型剤等の添加剤および重合開始剤と共に
、モノマーは溶解するが、重合体は溶解しない溶媒中に
溶解し、重合体の溶媒での分散性を安定させる分散安定
剤の存在下、攪拌しつつモノマーを析出、重合させてコ
ア粒子を得るものである。Further, instead of the emulsion polymerization method, the microparticles may be created using a dispersion polymerization method. Here, the dispersion polymerization method refers to dissolving monomers together with additives such as colorants and mold release agents, and polymerization initiators in a solvent in which the monomers are dissolved but the polymer is not. Core particles are obtained by precipitating and polymerizing monomers while stirring in the presence of a dispersion stabilizer that stabilizes dispersibility.
負帯電性樹脂粒子の製造
前記コア粒子を水系媒体中に懸濁させた懸濁液と、前記
微小粒子のエマルションまたは懸濁液とを混合し、つい
で前記コア粒子のガラス転移温度以上の温度て熱処理し
てコア粒子の表面に微小粒子を融着させる。Production of negatively charged resin particles A suspension obtained by suspending the core particles in an aqueous medium and an emulsion or suspension of the microparticles are mixed, and then heated to a temperature equal to or higher than the glass transition temperature of the core particles. Heat treatment is performed to fuse the microparticles to the surface of the core particles.
コア粒子の分散液と微小粒子のエマルションとの配合割
合は、双方の粒子径の比にもよるか、固形分換算で１０
０：０．１〜１００：２０であるのか適当てあり、微小
粒子かこの範囲よりも小なるときは、微小粒子によるコ
ア粒子の被覆か不充分であるために微小粒子によるコア
粒子の粒子間架橋か生して凝集体か発生してしまい、逆
にこの範囲より大なるときは微小粒子か余剰となり、除
去か煩雑となるはかりでなく、コア粒子表面に二層以上
の微小粒子か付着した場合には静電引力が不充分である
ためにトナー化した後にトナーから剥離するような弱い
付着粒子となり、いずれも好ましくない。The blending ratio of the core particle dispersion and the fine particle emulsion may depend on the ratio of the particle sizes of both, or may be 10% in terms of solid content.
It depends on whether the ratio is 0:0.1 to 100:20, but if the particles are smaller than this range, the coverage of the core particles with the microparticles is insufficient, and the particles between the core particles are not covered by the microparticles. Aggregates are generated due to cross-linking, and conversely, if the size is larger than this range, it becomes a small particle or surplus, and it is difficult to remove it. In some cases, the electrostatic attraction is insufficient, resulting in weakly adhered particles that peel off from the toner after being formed into a toner, which is not preferable.
熱処理温度は、コア粒子と微小粒子とを融着させるため
に、コア粒子のガラス転移温度（トナーの場合、約５０
〜８０°Ｃ）の近傍またはそれよりも上て行われる。The heat treatment temperature is set at the glass transition temperature of the core particles (approximately 50
~80°C) or above.
熱処理後、洗浄、濾過、乾燥して負帯電性樹脂粒子を得
る。After heat treatment, the particles are washed, filtered, and dried to obtain negatively charged resin particles.
かくして得られる負帯電性樹脂粒子は、これをトナーと
して利用するときは、粒径３〜２５μｍ、とくに８〜２
０μｍの複合球状粒子として得られ、すぐれた流動性、
帯電性、定着性およびクリーニング特性を示すものとな
る。When the negatively charged resin particles thus obtained are used as a toner, the particle size is 3 to 25 μm, particularly 8 to 2 μm.
Obtained as composite spherical particles of 0 μm, excellent fluidity,
It exhibits charging properties, fixing properties, and cleaning properties.
また、トナーとするときには、感光体を清浄化するため
の研磨剤を添加してもよい。研磨剤としては、例えはタ
ルク、カオリン、硫酸バリウムのほか、ケイ酸アルミニ
ウム、表面処理したケイ酸アルミニウム、二酸化チタン
、炭酸カルシウム、三酸化アンチモン、チタン酸バリウ
ム、チタン酸カルシウム、チタン酸ストロンチウム、酸
化マグ不ンウム、ケイ酸カルンウム、酸化亜鉛等が好ま
しく、特にコロイド状ノリ力、表面処理した疎水性シリ
カか好ましい。研磨剤、とくに疎水性ソリ力の添加によ
りトナー（現像剤）の流動性も良くなる。研磨剤の平均
粒径は１〜］００ｎｍ、とてにｌＯ〜３０ｎｍであるの
が好ましい。また、添加量はトナー１００重量部に対し
て０．０１〜１重量部であるのか好ましく、添加量か０
．０１重量部未満であるとトナーの流動性か劣り、また
１重量部を超えると感光体が傷つき易くなる傾向にある
。Further, when used as a toner, an abrasive for cleaning the photoreceptor may be added. Examples of abrasives include talc, kaolin, barium sulfate, as well as aluminum silicate, surface-treated aluminum silicate, titanium dioxide, calcium carbonate, antimony trioxide, barium titanate, calcium titanate, strontium titanate, and oxidized aluminum. Preferable are magnonium, carunium silicate, zinc oxide, etc., and particularly preferable are colloidal adhesive and surface-treated hydrophobic silica. The fluidity of the toner (developer) also improves by adding an abrasive, especially a hydrophobic warping force. The average particle diameter of the abrasive is preferably 1 to 00 nm, particularly 10 to 30 nm. Further, the amount added is preferably 0.01 to 1 part by weight per 100 parts by weight of toner, and the amount added is preferably 0.01 to 1 part by weight per 100 parts by weight of toner.
．． If the amount is less than 1 part by weight, the fluidity of the toner will be poor, and if it exceeds 1 part by weight, the photoreceptor will tend to be easily damaged.
また、トナーの電気抵抗を調整する目的でカーホンブラ
ック、酸化アルミニウム等をまふして使用してもよい。Further, in order to adjust the electrical resistance of the toner, carphone black, aluminum oxide, etc. may be used as a muff.
これらの電気抵抗調整剤はトナー１００重量部に対して
０．０１〜１重量部であるのか適当である。These electrical resistance regulators may be used in an appropriate amount of 0.01 to 1 part by weight per 100 parts by weight of the toner.
本発明の方法によって得られる電荷制御用樹脂粒子は、
表面の微小粒子により摩擦帯電等によって負の電荷を示
すので、静電荷偉現像用の負帯電性トナーとして好適に
使用できる。その際、樹脂粒子の帯電性は、コア粒子お
よび微小粒子にそれぞれ使用する水系媒体中で正の電荷
を存するモノマーまたは負の電荷を有するモノマーと他
のモノマーとの配合比を適宜変更することによって簡単
に制御することができる。The charge control resin particles obtained by the method of the present invention are:
Since the fine particles on the surface exhibit a negative charge due to triboelectric charging or the like, it can be suitably used as a negatively chargeable toner for electrostatic development. At that time, the chargeability of the resin particles can be controlled by appropriately changing the blending ratio of positively charged monomers or negatively charged monomers and other monomers in the aqueous medium used for the core particles and microparticles, respectively. Can be easily controlled.
また、光導電性材料を含存した感光性トナー等にも適用
可能であり、またその負帯電性を利用して静電塗料等の
他の用途にも使用可能である。It can also be applied to photosensitive toners containing photoconductive materials, and can also be used in other applications such as electrostatic paints by utilizing its negative chargeability.
なお、以上の説明では、コア粒子か正荷電を有し、微小
粒子か負荷電を有する構成としたか、これとは逆にコア
粒子か負荷電を有し、微小粒子か正荷電を有する構成と
してもよい。この場合は正帯電性樹脂粒子となる。In the above explanation, the core particles have a positive charge and the microparticles have a negative charge, or conversely, the core particles have a negative charge and the microparticles have a positive charge. You can also use it as In this case, the resin particles are positively charged.
また、コア粒子および微小粒子の両方を懸濁重合法にて
作成してもよい。Furthermore, both the core particles and the microparticles may be produced by a suspension polymerization method.
また、コア粒子および微小粒子に正または負の電荷を付
与する方法として、正または負の電荷を有するモノマー
または重合開始剤を使用したか、重合時または重合後に
それぞれカチオン性界面活性剤およびアニオン性界面活
性剤を添加してもよい。カチオン性界面活性剤としては
、例えはアルキルアミン、アルキルエチレンノアミン、
アルキルトリメチルシアミン、アルキルピリジニウム、
アルキルジメチルヘンンルアンモニウム等があげられる
。また、アニオン系界面活性剤としては、例えばアルキ
ル硫酸ナトリウム、ポリオキソエチしンアルキルアリル
スルホン酸ナトリウム、アルキルノフＬニルエーテルジ
スルホン酸ナトリウム、アルキルベンセンスルホン酸ナ
トリウム等があげられる。In addition, as a method of imparting positive or negative charges to core particles and microparticles, monomers or polymerization initiators with positive or negative charges were used, or cationic surfactants and anionic surfactants were used during or after polymerization, respectively. Surfactants may also be added. Examples of cationic surfactants include alkylamines, alkylethylenenoamines,
Alkyltrimethylcyamine, alkylpyridinium,
Examples include alkyldimethylhenruammonium. Examples of the anionic surfactant include sodium alkyl sulfate, sodium polyoxoethylene alkylaryl sulfonate, sodium alkylnovyl ether disulfonate, and sodium alkylbensene sulfonate.
さらに、電荷制御のために、コア粒子または微小粒子中
に負帯電性または正帯電性電荷制御用重合体（または共
重合体）を含有させてもよい。Furthermore, for charge control, a negatively chargeable or positively chargeable charge control polymer (or copolymer) may be contained in the core particles or fine particles.
（以下余白）
〈実施例〉
以下に実施例および比較例をあげて本発明の電子写真用
トナーを説明する。(The following is a blank space) <Example> The electrophotographic toner of the present invention will be described below with reference to Examples and Comparative Examples.
負帯電性電荷制御共重合体の合成１
下記成分を混合し、窒素雰囲気下、緩攪拌しなから８０
°Ｃで１２時間重合反応させた。Synthesis of negatively chargeable charge control copolymer 1 Mix the following components and stir gently under nitrogen atmosphere until 80%
The polymerization reaction was carried out at °C for 12 hours.
（成分） （重量部）スチレン
６０α−フェニルヒニルホスホン
酸 ４０２．２−アゾビス（２，４−ジメチ
ルバレロニトリル）１０
メチルアルコール ４００得られた重合物
をエバポレーションにより乾燥・粉末化し負帯電性電荷
制御共重合体ｌを得た。(Ingredients) (Parts by weight) Styrene
60α-phenylhinylphosphonic acid 402.2-Azobis(2,4-dimethylvaleronitrile) 10 Methyl alcohol 400 The obtained polymer was dried and powdered by evaporation to obtain a negatively charged charge control copolymer l. .
負帯電性電荷制御共重合体の合成２
下記成分を混合し、窒素雰囲気下、緩攪拌しなから６０
°Ｃて１２時間重合反応させた。Synthesis of negatively chargeable charge control copolymer 2 Mix the following components and stir gently under nitrogen atmosphere for 60 minutes.
The polymerization reaction was carried out at °C for 12 hours.
（以下余白）
（成分） （重量部）スチレン
９０スチレンスルホン酸ナトリ
ウム １０アブヒスイソブチロニトリル １０ポ
リアクリル酸 １０イソプロピルア、
ルコール ６００水
２００得られた重合物の媒体を遠
心分離によりメタノールに置換した後、エバポレーショ
ンにより乾燥・粉末化し負帯電性電荷制御共重合体２を
得た。(Left below) (Ingredients) (Parts by weight) Styrene
90 Sodium styrene sulfonate 10 Abhis isobutyronitrile 10 Polyacrylic acid 10 Isopropyla,
Lecole 600 water
The medium of the obtained polymer was replaced with methanol by centrifugation, and then dried and powdered by evaporation to obtain negatively chargeable charge control copolymer 2.
コア粒子の合成例１
水８００重量部に懸濁安定剤としてリン酸三カルソウム
（太平化学産業社製の商品名ＴＣＰ−１０、固形分濃度
１０％）の１００重量部およびラウリル硫酸ナトリウム
０．０１２重量部を加えた連続相に下記成分の混合物を
投入し、ホモミキサーを用いて造粒し、緩攪拌下、８０
°Ｃにて８時間重合反応を行った。Synthesis Example 1 of Core Particles 100 parts by weight of tricalcium phosphate (trade name TCP-10, manufactured by Taihei Kagaku Sangyo Co., Ltd., solid content concentration 10%) as a suspension stabilizer in 800 parts by weight of water and 0.012 parts by weight of sodium lauryl sulfate A mixture of the following components was added to the continuous phase to which parts by weight had been added, granulated using a homo mixer, and 80%
The polymerization reaction was carried out at °C for 8 hours.
（成分） （重量部）スチレン
７５２−エチルペキン
ルメタクリレート １５
ンメチルアミノエチ
ルメタクリレート ＩＯ
ジビニルベンゼン ０７２−エチレン
グリコ−
ルジメタクリレート １５含金属染料（電
荷制御剤） ３（オリエント化学社製の
ホントロンＳ−３４）
カーホンブラック ５
（三菱化成社製の九ＩＡ−１００）
２．２°−アゾビス（２，４−ジメチ
ルバレロニトリル）（重合開始剤） ３２．２−アゾ
ビス（２−メチルブ
チロニトリル）（重合開始剤） １得られた重合
物を水洗、濾過、再分散を３度繰り返すことにより正帯
電コア粒子懸濁液Ｊを得た。(Ingredients) (Parts by weight) Styrene
752-Ethylpequinyl methacrylate 15-methylaminoethyl methacrylate IO Divinylbenzene 072-Ethylene glycol dimethacrylate 15 Metal-containing dye (charge control agent) 3 (Hontron S-34 manufactured by Orient Chemical Co., Ltd.) Carphone black 5 (Mitsubishi Chemical Co., Ltd.) 9 IA-100 manufactured by Co., Ltd.) 2.2°-azobis(2,4-dimethylvaleronitrile) (polymerization initiator) 32. 2-azobis(2-methylbutyronitrile) (polymerization initiator) 1 obtained Positively charged core particle suspension J was obtained by repeating washing, filtration, and redispersion of the polymer three times.
コア粒子の合成例２
コア粒子の合成例１て用いたツメチルアミノエチルメタ
クリレ−８１０重量部に代えて、ノエチルアミノブロピ
ルメタクリレート１０重量部を用いたほかは上記コア粒
子の合成例１と同様にして正帯電コア粒子懸濁液２を得
た。Synthesis Example 2 of Core Particles Synthesis Example 1 of Core Particles Above, except that 10 parts by weight of noethylaminopropyl methacrylate was used in place of 810 parts by weight of trimethylaminoethyl methacrylate used in Synthesis Example 1 of Core Particles. Positively charged core particle suspension 2 was obtained in the same manner as above.
コア粒子の合成例３
水８００重量部に懸濁安定剤としてリン酸三カルノウム
（太平化学産業社製の商品名ＴＣＰ−１０、固形分濃度
ｌＯ％）の１００重量部およびラウリル硫酸ナトリウム
００１２重量部を加えた連続相に下記成分の混合物を投
入し、ホモミキサーを用いて造粒し、緩攪拌下、８０°
Ｃにて８時間重合反応を行った。Synthesis Example 3 of Core Particles 100 parts by weight of tricarnoum phosphate (trade name TCP-10, manufactured by Taihei Kagaku Sangyo Co., Ltd., solid content concentration 10%) as a suspension stabilizer in 800 parts by weight of water and 12 parts by weight of sodium lauryl sulfate. A mixture of the following components was added to the continuous phase, granulated using a homomixer, and heated at 80° with gentle stirring.
The polymerization reaction was carried out at C for 8 hours.
（以下余白ン
（成分） （重量部）スチレン
７５２−エチルへキン
ルメタクリレート １５負帯電性電荷制
御共重合体１ １０
ジヒニルペンセン ０７２−エチレン
グリコ−
ルソメタクリレート １． ５含金属染
料（電荷制御剤） ２（オリエント化学社製
のホントロンＮ−１１）カーホンブラック
５（三菱化成社製のＭＡ−１００）
２．２−アゾビス（２，４−ツメチ
ルバレロニトリル）（重合開始剤） ３２．２°−
アゾヒス（２−メチルブ
チロニトリル）（重合開始剤） １得られた重
合物を水洗、濾過、再分散を３度繰り返すことにより負
帯電コア粒子暫濁液３を得た。(Hereinafter the margin is (Ingredients) (Parts by weight) Styrene
752-Ethylhequinyl methacrylate 15 Negatively chargeable charge control copolymer 1 10 Dihinyl pentene 072-Ethylene glycol methacrylate 1. 5 Metal-containing dye (charge control agent) 2 (Hontron N-11 manufactured by Orient Chemical Co., Ltd.) Carphone black
5 (MA-100 manufactured by Mitsubishi Kasei Corporation) 2.2-azobis(2,4-trimethylvaleronitrile) (polymerization initiator) 32.2°-
Azohis (2-methylbutyronitrile) (polymerization initiator) 1 The obtained polymer was washed with water, filtered, and redispersed three times to obtain a negatively charged core particle suspension 3.
コア粒子の合成例４
コア粒子の合成例３て用いた負帯電性電荷制御共重合体
ｌの１０重量部に代えて、負帯電性電荷制御共重合体２
の３重量部を用いたほかは上記コア粒子の合成例３と同
様にして負帯電コア粒子懸濁液４を得た。Core particle synthesis example 4 In place of 10 parts by weight of the negatively chargeable charge control copolymer 1 used in core particle synthesis example 3, negatively chargeable charge control copolymer 2 was added.
A negatively charged core particle suspension 4 was obtained in the same manner as in Core Particle Synthesis Example 3 except that 3 parts by weight of .
微小粒子の合成例１
下記成分を混合し、緩攪拌下、８０°Ｃて６時間無乳化
剤乳化重合反応を行うことにより、負帯電樹脂微粒子エ
マル７ョン１を得た。Synthesis Example 1 of Fine Particles Negatively charged resin fine particle emulsion 7 was obtained by mixing the following components and carrying out an emulsifier-free emulsion polymerization reaction at 80° C. for 6 hours with gentle stirring.
（成分） （重量部９スチレン
７２２−エチルへキノルメタ
クリレート ２５スチレンスルホ
ン酸ナトリウム ３水
９００過硫酸カリウム（重合開始剤
） １微小粒子の合成例２
下記成分を混合し、緩攪拌下、８０°Ｃて６時間重合反
応を行うことにより、正帯電樹脂微粒子エマルション２
を得た。(Ingredients) (Part by weight 9 styrene
722-ethyl quinol methacrylate 25 Sodium styrene sulfonate 3 water
900 Potassium persulfate (polymerization initiator) 1 Synthesis example of microparticles 2 By mixing the following components and carrying out a polymerization reaction at 80°C for 6 hours with gentle stirring, positively charged resin microparticle emulsion 2
I got it.
（成分） （重量部）スチレン
７２２−エチルへキンルメタ
ク リ し − ト
２５ンメチルアミノエチルメ
タフリレート ３水
９００アゾヒス（
２−アミジノプ
ロパン）塩酸基本 １
本チャージ性重合開始剤
実施例１
正帯電コア粒子懸濁液ｌの１００重量部と負帯電樹脂微
粒子エマルション１の３重量部とを混合し、１２規定の
塩酸２０重量部を添加し、緩攪拌下にて７０°Ｃて１時
間熱処理を行うことによりコア粒子の表面に樹脂微粒子
を固着させた。これを洗浄、濾過、乾燥、解砕して、ト
ナー粒子を得た。(Ingredients) (Parts by weight) Styrene
722-Ethyl methacrylate
25-methylaminoethylmethafrylate 3 water
900 Azohis (
2-amidinopropane) Hydrochloric acid basic 1 Chargeable polymerization initiator Example 1 100 parts by weight of positively charged core particle suspension 1 and 3 parts by weight of negatively charged resin fine particle emulsion 1 were mixed, and 12N hydrochloric acid 20 Parts by weight were added and heat treated at 70°C for 1 hour under gentle stirring to fix the resin fine particles on the surface of the core particles. This was washed, filtered, dried and crushed to obtain toner particles.
このトナー粒子の粒度分布をコールタ−カウンタを用い
て測定したところ、体積基準のメジアン径Ｄ ｉｏは１
０．８μｍてノヤープな粒度分布を有するものてあった
。When the particle size distribution of the toner particles was measured using a Coulter counter, the volume-based median diameter D io was 1.
Some had a uniform particle size distribution of 0.8 μm.
得られたトナー１００重量部に対して０．１重量部の疎
水性ノリカ微粉末を混合し、さらにノリコーン樹脂被覆
されたフェライトキャリアと混合して、トナー濃度か３
，８％の現像剤を調製した。電子写真複写機ＤＣ−２５
８５（三田工業株式会社製の商品名）により、得られた
現像剤を用いて２０００枚の連続複写試験を行い、画質
および現像剤の耐久性についで評価した。また、高温高
湿環境下（温度３０°Ｃ１湿度８０％）にて５００枚連
続複写後の画質から耐湿性を評価した。これらの試験結
果を第１表に示す。0.1 part by weight of hydrophobic Norica fine powder was mixed with 100 parts by weight of the obtained toner, and further mixed with a ferrite carrier coated with Noricone resin to give a toner concentration of 3.
, 8% developer was prepared. Electrophotocopy machine DC-25
85 (trade name, manufactured by Sanda Kogyo Co., Ltd.), a continuous copying test of 2,000 sheets was conducted using the obtained developer, and the image quality and durability of the developer were then evaluated. In addition, the moisture resistance was evaluated based on the image quality after 500 sheets were continuously copied under a high temperature and high humidity environment (temperature: 30° C., humidity: 80%). The results of these tests are shown in Table 1.
実施例２
実施例１て用いた正帯電コア粒子Ｐ濁液ｌの１００重量
部に代えて正帯電コア粒子懸濁液２の１００重量部を用
いたほかは、実施例１と同様にしてトナー粒子を得た。Example 2 A toner was prepared in the same manner as in Example 1, except that 100 parts by weight of positively charged core particle suspension 2 was used in place of 100 parts by weight of positively charged core particle P suspension L used in Example 1. Particles were obtained.
このトナー粒子のメツアン径Ｄ 、ａｏは１１，４μｍ
でシャープな粒度分布を有するものであった。また、実
施例１と同様にして、このトナーの性能評価を行った。The methuan diameter D and ao of this toner particle is 11.4 μm
It had a sharp particle size distribution. Further, the performance of this toner was evaluated in the same manner as in Example 1.
その試験結果を第１表に示す。The test results are shown in Table 1.
実施例３
実施例】て用いた正帯電コア粒子懸濁液１の１００重量
部に代えて負帯電コア粒子懸濁液３の１００重量部を用
い、かつ実施例１て用いた負帯電微小粒子エマルション
１に代えて正帯電微小粒子エマルション２の３重量部を
用いたほかは実施例Ｉと同様にしてトナー粒子を得た。Example 3 100 parts by weight of negatively charged core particle suspension 3 was used in place of 100 parts by weight of positively charged core particle suspension 1 used in Example 1, and the negatively charged fine particles used in Example 1 were Toner particles were obtained in the same manner as in Example I except that 3 parts by weight of positively charged fine particle emulsion 2 was used in place of emulsion 1.
このトナー粒子のメンアン径Ｉ）ｓｏは１０．５μｍで
シャープな粒度分布を有するものであった。The toner particles had a mean diameter I)so of 10.5 μm and a sharp particle size distribution.
また、得られたトナー１００重量部に対して０．１重量
部の疎水性ンリカ微粉末を混合し、さらにノリコーン樹
脂被覆されたフェライトキャリアと混合して、トナー濃
度か３．８％の現像剤を調製した。In addition, 0.1 parts by weight of hydrophobic phosphoric acid fine powder was mixed with 100 parts by weight of the obtained toner, and further mixed with a ferrite carrier coated with Noricone resin to form a developer with a toner concentration of 3.8%. was prepared.
電子写真方式プリンターＬＰＸ−１（三田工業株式会社
製の商品名）を用いて、トナーの性能評価を実施例１と
同様にして行った。その試験結果を第１表に示す。The toner performance was evaluated in the same manner as in Example 1 using an electrophotographic printer LPX-1 (trade name, manufactured by Sanda Kogyo Co., Ltd.). The test results are shown in Table 1.
実施例４
実施例１て用いた正帯電コア粒子懸濁液３の１００重量
部に代えて負帯電コア粒子懸濁液４の１００重量部を用
い、かつ実施例１て用いた負帯電微小粒子エマル７ョン
１に代えて正帯電微小粒子エマルション２の３重量部を
用いたほかは実施例１と同様にしてトナー粒子を得た。Example 4 100 parts by weight of the positively charged core particle suspension 3 used in Example 1 was replaced with 100 parts by weight of the negatively charged core particle suspension 4, and the negatively charged fine particles used in Example 1 were used. Toner particles were obtained in the same manner as in Example 1, except that Emulsion 7 was replaced with 3 parts by weight of positively charged fine particle emulsion 2.
このトナー粒子のメジアン径Ｄ５゜は１０．２μｍでシ
ャープな粒度分布を有するものであった。また、実施例
】と同様にして、このトナーの性能評価を行った。その
試験結果を第１表に示す。The toner particles had a median diameter D5° of 10.2 μm and a sharp particle size distribution. Further, the performance of this toner was evaluated in the same manner as in Example. The test results are shown in Table 1.
比較例１
水８００重量部に分散安定剤としてリン酸三カルノウム
（太平化学産業社製の商品名ＴＣＰ−１０、固形分濃度
ＩＯ％）の１００重量部およびラウリル硫酸ナトリウム
００１２重量部を加えた連続相に下記成分の混合物を投
入し、ホモミキサーを用いて造粒し、緩攪拌下、８０°
Ｃにて８時間重合反応を行った。Comparative Example 1 100 parts by weight of tricarnoum phosphate (trade name: TCP-10, manufactured by Taihei Kagaku Sangyo Co., Ltd., solid content concentration IO%) and 0.012 parts by weight of sodium lauryl sulfate were added as a dispersion stabilizer to 800 parts by weight of water. A mixture of the following components was added to the phase, granulated using a homomixer, and heated at 80° with gentle stirring.
The polymerization reaction was carried out at C for 8 hours.
（成分） （重量部）スチレン
７５２−エチルへキン
ルメタクリレート １５負帯電性電荷制
御共重合体１ １Ｃ＋ジヒニルヘンセン
０７２−エチレングリコ−
ルジメタクリレート １５含金属染料（
を荷割面剤） ２（オリエント化学社製の
ホントロンＳ−３４）
カーホンブラック ５（三菱化成社製
のＭＡ−１００）
２．２゛−アゾヒス（２，４−ジメチ
ルバレロニトリル）（重合開始剤）３
２．２−アブビス（２−メチルブ
チロニトリル）（重合開始剤） １得られた重合
物を水洗、濾過、乾燥することによりトナー粒子を得た
。(Ingredients) (Parts by weight) Styrene
752-Ethyl hequinyl methacrylate 15 Negatively chargeable charge control copolymer 1 1C+dihinylhensen
072-Ethylene glycol dimethacrylate 15 Metal-containing dye (
2 (Hontron S-34 manufactured by Orient Chemical Co., Ltd.) Carphone Black 5 (MA-100 manufactured by Mitsubishi Kasei Co., Ltd.) 2.2゛-Azohis (2,4-dimethylvaleronitrile) (polymerization initiation Agent) 3 2.2-abbis(2-methylbutyronitrile) (polymerization initiator) 1 The obtained polymer was washed with water, filtered, and dried to obtain toner particles.
このトナー粒子の性能評価を実施例１と同様にして、二
のトナーの性能評価を行ったところ、第１表に示すよう
な試験結果か得られた。When the performance of this toner particle was evaluated in the same manner as in Example 1, the performance of the second toner was evaluated, and the test results shown in Table 1 were obtained.
比較例２
実施例１において、塩酸を使用しなかったほかは実施例
１と同様にしてトナー粒子を得た。Comparative Example 2 Toner particles were obtained in the same manner as in Example 1 except that hydrochloric acid was not used.
このトナー粒子の表面には、微小粒子か付着していなか
った。また、実施例１と同様にして、このトナーの性能
評価を行ったところ、はとんど帯電性を示さず、トナー
か飛散した。No fine particles were attached to the surface of this toner particle. Further, when the performance of this toner was evaluated in the same manner as in Example 1, it showed almost no chargeability and some of the toner was scattered.
第１表において、初期画質と複写後の画質は以下の基準
で評価した。In Table 1, the initial image quality and the image quality after copying were evaluated based on the following criteria.
○−かぶりなく、良好な画像である。○ - Good image with no fog.
△ わずかにかふりか見られる。△ Slight smudges can be seen.
ム かふりか多い × 現像スリーブよりトナーか飛散する。There are a lot of mukafurika × Toner scatters from the developing sleeve.
（以下余白）
表から明らかなごとく、実施例１〜４て得たトナー粒子
は、帯電性にすぐれ、初期画質はもとより多数枚複写後
の画質の低下もなく、耐湿性にもすぐれていた。これに
対して、比較例１てはとぐに耐湿性に劣っており、比較
例２ては微小粒子かコア粒子に付着していないため、帯
電性に劣っていた。(Hereafter, blank space) As is clear from the table, the toner particles obtained in Examples 1 to 4 had excellent charging properties, no deterioration in initial image quality or image quality after copying a large number of sheets, and had excellent moisture resistance. On the other hand, Comparative Example 1 was extremely poor in moisture resistance, and Comparative Example 2 was poor in chargeability because the fine particles were not attached to the core particles.
〈発明の効果〉
本発明の電荷制御用樹脂粒子の製造方法によねは、コア
粒子および樹脂微粒子かそれぞれ水系媒体中で正および
負に荷電するので、両者の付着か強固になり、摩擦等に
対する耐久性にすぐれたものになる。<Effects of the Invention> According to the method for producing resin particles for charge control of the present invention, the core particles and the resin fine particles are respectively positively and negatively charged in an aqueous medium, so that the adhesion between the two becomes strong and resistant to friction, etc. It becomes highly durable.
また、本発明の電荷制御用樹脂粒子をトナーとして利用
するときは、帯電性にすぐれ、かつ耐湿性にもすぐれて
いるという効果かある。Furthermore, when the charge control resin particles of the present invention are used as a toner, they have the advantage of having excellent charging properties and moisture resistance.
Claims (1)
のコア粒子と微小粒子とを熱処理してコア粒子の表面に
微小粒子を融着させる電荷制御用樹脂粒子の製造方法に
おいて、 前記懸濁重合を懸濁安定剤として難水溶性無機粉末を用
いて行ない、ついで生成重合体の懸濁液を、前記難水溶
性無機粉末を溶解させるｐＨ値に調節した後、前記熱処
理を行うことを特徴とする電荷制御用樹脂粒子の製造方
法。[Scope of Claims] 1. A method for producing resin particles for charge control, in which core particles and microparticles of resin having opposite charges are heat-treated in an aqueous medium to fuse the microparticles to the surface of the core particles. , the suspension polymerization is carried out using a poorly water-soluble inorganic powder as a suspension stabilizer, and then the resulting polymer suspension is adjusted to a pH value that dissolves the poorly water-soluble inorganic powder, and then the heat treatment is carried out. 1. A method for producing resin particles for charge control, characterized in that:
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2320196A JPH04194868A (en) | 1990-11-22 | 1990-11-22 | Manufacture of electric charge controlling resin particle |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2320196A JPH04194868A (en) | 1990-11-22 | 1990-11-22 | Manufacture of electric charge controlling resin particle |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH04194868A true JPH04194868A (en) | 1992-07-14 |
Family
ID=18118778
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2320196A Pending JPH04194868A (en) | 1990-11-22 | 1990-11-22 | Manufacture of electric charge controlling resin particle |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH04194868A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH10207114A (en) * | 1997-01-24 | 1998-08-07 | Nippon Zeon Co Ltd | Developer |
| JP2001272821A (en) * | 2001-02-16 | 2001-10-05 | Fujitsu Ltd | Method for manufacturing toner |
| US7553600B2 (en) | 2005-09-29 | 2009-06-30 | Brother Kogyo Kabushiki Kaisha | Method for producing toner and positively chargeable non-magnetic single component toner |
-
1990
- 1990-11-22 JP JP2320196A patent/JPH04194868A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH10207114A (en) * | 1997-01-24 | 1998-08-07 | Nippon Zeon Co Ltd | Developer |
| JP2001272821A (en) * | 2001-02-16 | 2001-10-05 | Fujitsu Ltd | Method for manufacturing toner |
| US7553600B2 (en) | 2005-09-29 | 2009-06-30 | Brother Kogyo Kabushiki Kaisha | Method for producing toner and positively chargeable non-magnetic single component toner |
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