JPH01277254A - Manufacture of magnetic toner - Google Patents
Manufacture of magnetic tonerInfo
- Publication number
- JPH01277254A JPH01277254A JP63108085A JP10808588A JPH01277254A JP H01277254 A JPH01277254 A JP H01277254A JP 63108085 A JP63108085 A JP 63108085A JP 10808588 A JP10808588 A JP 10808588A JP H01277254 A JPH01277254 A JP H01277254A
- Authority
- JP
- Japan
- Prior art keywords
- toner
- magnetic
- polymerization
- magnetic field
- particles
- 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 abstract description 16
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 34
- 238000010557 suspension polymerization reaction Methods 0.000 claims description 5
- 239000002245 particle Substances 0.000 abstract description 37
- 239000006249 magnetic particle Substances 0.000 abstract description 31
- 239000000178 monomer Substances 0.000 abstract description 26
- 239000000203 mixture Substances 0.000 abstract description 14
- 238000000034 method Methods 0.000 abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 9
- 239000003795 chemical substances by application Substances 0.000 abstract description 8
- 238000003756 stirring Methods 0.000 abstract description 8
- 239000006185 dispersion Substances 0.000 abstract description 6
- 239000003505 polymerization initiator Substances 0.000 abstract description 6
- 239000003086 colorant Substances 0.000 abstract description 5
- 239000000725 suspension Substances 0.000 abstract description 5
- 239000003381 stabilizer Substances 0.000 abstract description 4
- 229920000642 polymer Polymers 0.000 abstract description 3
- 238000005453 pelletization Methods 0.000 abstract 1
- 238000011161 development Methods 0.000 description 11
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 7
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 6
- -1 conventionally Substances 0.000 description 6
- 238000005469 granulation Methods 0.000 description 6
- 230000003179 granulation Effects 0.000 description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 5
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 5
- 125000000217 alkyl group Chemical group 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 5
- 230000005484 gravity Effects 0.000 description 5
- 239000000049 pigment Substances 0.000 description 5
- 239000000843 powder Substances 0.000 description 5
- MYRTYDVEIRVNKP-UHFFFAOYSA-N 1,2-Divinylbenzene Chemical compound C=CC1=CC=CC=C1C=C MYRTYDVEIRVNKP-UHFFFAOYSA-N 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 239000004372 Polyvinyl alcohol Substances 0.000 description 3
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 3
- 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 3
- 239000000975 dye Substances 0.000 description 3
- 125000005843 halogen group Chemical group 0.000 description 3
- 229910017053 inorganic salt Inorganic materials 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229920002451 polyvinyl alcohol Polymers 0.000 description 3
- YGSDEFSMJLZEOE-UHFFFAOYSA-N salicylic acid Chemical compound OC(=O)C1=CC=CC=C1O YGSDEFSMJLZEOE-UHFFFAOYSA-N 0.000 description 3
- 229920001567 vinyl ester resin Polymers 0.000 description 3
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 3
- 229920002554 vinyl polymer Polymers 0.000 description 3
- VXNZUUAINFGPBY-UHFFFAOYSA-N 1-Butene Chemical compound CCC=C VXNZUUAINFGPBY-UHFFFAOYSA-N 0.000 description 2
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 description 2
- KAKZBPTYRLMSJV-UHFFFAOYSA-N Butadiene Chemical compound C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 description 2
- SOGAXMICEFXMKE-UHFFFAOYSA-N Butylmethacrylate Chemical compound CCCCOC(=O)C(C)=C SOGAXMICEFXMKE-UHFFFAOYSA-N 0.000 description 2
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-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
- QYKIQEUNHZKYBP-UHFFFAOYSA-N Vinyl ether Chemical compound C=COC=C QYKIQEUNHZKYBP-UHFFFAOYSA-N 0.000 description 2
- 239000012736 aqueous medium Substances 0.000 description 2
- 239000008346 aqueous phase Substances 0.000 description 2
- AYJRCSIUFZENHW-DEQYMQKBSA-L barium(2+);oxomethanediolate Chemical compound [Ba+2].[O-][14C]([O-])=O AYJRCSIUFZENHW-DEQYMQKBSA-L 0.000 description 2
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 description 2
- 125000004432 carbon atom Chemical group C* 0.000 description 2
- 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 2
- 229910017052 cobalt Inorganic materials 0.000 description 2
- 239000010941 cobalt Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 230000002950 deficient Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- QDOXWKRWXJOMAK-UHFFFAOYSA-N dichromium trioxide Chemical compound O=[Cr]O[Cr]=O QDOXWKRWXJOMAK-UHFFFAOYSA-N 0.000 description 2
- 150000002430 hydrocarbons Chemical group 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 150000005673 monoalkenes Chemical class 0.000 description 2
- FJKROLUGYXJWQN-UHFFFAOYSA-N papa-hydroxy-benzoic acid Natural products OC(=O)C1=CC=C(O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-N 0.000 description 2
- 108091008695 photoreceptors Proteins 0.000 description 2
- 239000001054 red pigment Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229960004889 salicylic acid Drugs 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- OSNILPMOSNGHLC-UHFFFAOYSA-N 1-[4-methoxy-3-(piperidin-1-ylmethyl)phenyl]ethanone Chemical compound COC1=CC=C(C(C)=O)C=C1CN1CCCCC1 OSNILPMOSNGHLC-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
- FFRBMBIXVSCUFS-UHFFFAOYSA-N 2,4-dinitro-1-naphthol Chemical compound C1=CC=C2C(O)=C([N+]([O-])=O)C=C([N+]([O-])=O)C2=C1 FFRBMBIXVSCUFS-UHFFFAOYSA-N 0.000 description 1
- XMNIXWIUMCBBBL-UHFFFAOYSA-N 2-(2-phenylpropan-2-ylperoxy)propan-2-ylbenzene Chemical compound C=1C=CC=CC=1C(C)(C)OOC(C)(C)C1=CC=CC=C1 XMNIXWIUMCBBBL-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
- JFMYRCRXYIIGBB-UHFFFAOYSA-N 2-[(2,4-dichlorophenyl)diazenyl]-n-[4-[4-[[2-[(2,4-dichlorophenyl)diazenyl]-3-oxobutanoyl]amino]-3-methylphenyl]-2-methylphenyl]-3-oxobutanamide Chemical compound C=1C=C(C=2C=C(C)C(NC(=O)C(N=NC=3C(=CC(Cl)=CC=3)Cl)C(C)=O)=CC=2)C=C(C)C=1NC(=O)C(C(=O)C)N=NC1=CC=C(Cl)C=C1Cl JFMYRCRXYIIGBB-UHFFFAOYSA-N 0.000 description 1
- QTSNFLIDNYOATQ-UHFFFAOYSA-N 2-[(4-chloro-2-nitrophenyl)diazenyl]-n-(2-chlorophenyl)-3-oxobutanamide Chemical compound C=1C=CC=C(Cl)C=1NC(=O)C(C(=O)C)N=NC1=CC=C(Cl)C=C1[N+]([O-])=O QTSNFLIDNYOATQ-UHFFFAOYSA-N 0.000 description 1
- LTHJXDSHSVNJKG-UHFFFAOYSA-N 2-[2-[2-[2-(2-methylprop-2-enoyloxy)ethoxy]ethoxy]ethoxy]ethyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OCCOCCOCCOCCOC(=O)C(C)=C LTHJXDSHSVNJKG-UHFFFAOYSA-N 0.000 description 1
- WDQMWEYDKDCEHT-UHFFFAOYSA-N 2-ethylhexyl 2-methylprop-2-enoate Chemical compound CCCCC(CC)COC(=O)C(C)=C WDQMWEYDKDCEHT-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
- HNNQYHFROJDYHQ-UHFFFAOYSA-N 3-(4-ethylcyclohexyl)propanoic acid 3-(3-ethylcyclopentyl)propanoic acid Chemical compound CCC1CCC(CCC(O)=O)C1.CCC1CCC(CCC(O)=O)CC1 HNNQYHFROJDYHQ-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
- LVOJOIBIVGEQBP-UHFFFAOYSA-N 4-[[2-chloro-4-[3-chloro-4-[(5-hydroxy-3-methyl-1-phenylpyrazol-4-yl)diazenyl]phenyl]phenyl]diazenyl]-5-methyl-2-phenylpyrazol-3-ol Chemical compound CC1=NN(C(O)=C1N=NC1=CC=C(C=C1Cl)C1=CC(Cl)=C(C=C1)N=NC1=C(O)N(N=C1C)C1=CC=CC=C1)C1=CC=CC=C1 LVOJOIBIVGEQBP-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
- 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
- 239000004342 Benzoyl peroxide Substances 0.000 description 1
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 229910052684 Cerium Inorganic materials 0.000 description 1
- REEFSLKDEDEWAO-UHFFFAOYSA-N Chloraniformethan Chemical compound ClC1=CC=C(NC(NC=O)C(Cl)(Cl)Cl)C=C1Cl REEFSLKDEDEWAO-UHFFFAOYSA-N 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
- WOBHKFSMXKNTIM-UHFFFAOYSA-N Hydroxyethyl methacrylate Chemical compound CC(=C)C(=O)OCCO WOBHKFSMXKNTIM-UHFFFAOYSA-N 0.000 description 1
- YIVJZNGAASQVEM-UHFFFAOYSA-N Lauroyl peroxide Chemical compound CCCCCCCCCCCC(=O)OOC(=O)CCCCCCCCCCC YIVJZNGAASQVEM-UHFFFAOYSA-N 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
- 239000004698 Polyethylene Substances 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 description 1
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 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
- GZHZIMFFZGAOGY-UHFFFAOYSA-N [O-2].[Fe+2].[La+3] Chemical compound [O-2].[Fe+2].[La+3] GZHZIMFFZGAOGY-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
- HZEWFHLRYVTOIW-UHFFFAOYSA-N [Ti].[Ni] Chemical compound [Ti].[Ni] HZEWFHLRYVTOIW-UHFFFAOYSA-N 0.000 description 1
- 239000006230 acetylene black Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 239000000654 additive Substances 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
- AOADSHDCARXSGL-ZMIIQOOPSA-M alkali blue 4B Chemical compound CC1=CC(/C(\C(C=C2)=CC=C2NC2=CC=CC=C2S([O-])(=O)=O)=C(\C=C2)/C=C/C\2=N\C2=CC=CC=C2)=CC=C1N.[Na+] AOADSHDCARXSGL-ZMIIQOOPSA-M 0.000 description 1
- 125000003545 alkoxy group Chemical group 0.000 description 1
- XYLMUPLGERFSHI-UHFFFAOYSA-N alpha-Methylstyrene Chemical compound CC(=C)C1=CC=CC=C1 XYLMUPLGERFSHI-UHFFFAOYSA-N 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
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- 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
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000000987 azo dye Substances 0.000 description 1
- HEQCHSSPWMWXBH-UHFFFAOYSA-L barium(2+) 1-[(2-carboxyphenyl)diazenyl]naphthalen-2-olate Chemical compound [Ba++].Oc1ccc2ccccc2c1N=Nc1ccccc1C([O-])=O.Oc1ccc2ccccc2c1N=Nc1ccccc1C([O-])=O HEQCHSSPWMWXBH-UHFFFAOYSA-L 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
- 235000019400 benzoyl peroxide Nutrition 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000001055 blue pigment Substances 0.000 description 1
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-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
- CXKCTMHTOKXKQT-UHFFFAOYSA-N cadmium oxide Inorganic materials [Cd]=O CXKCTMHTOKXKQT-UHFFFAOYSA-N 0.000 description 1
- CJOBVZJTOIVNNF-UHFFFAOYSA-N cadmium sulfide Chemical compound [Cd]=S CJOBVZJTOIVNNF-UHFFFAOYSA-N 0.000 description 1
- HTUDBOWEKWIOCZ-UHFFFAOYSA-N cadmium(2+) mercury(1+) sulfide Chemical compound [S-2].[Cd+2].[Hg+] HTUDBOWEKWIOCZ-UHFFFAOYSA-N 0.000 description 1
- CFEAAQFZALKQPA-UHFFFAOYSA-N cadmium(2+);oxygen(2-) Chemical compound [O-2].[Cd+2] CFEAAQFZALKQPA-UHFFFAOYSA-N 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 239000001506 calcium phosphate Substances 0.000 description 1
- 229910000389 calcium phosphate Inorganic materials 0.000 description 1
- 235000011010 calcium phosphates Nutrition 0.000 description 1
- 159000000007 calcium salts Chemical class 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- ZMIGMASIKSOYAM-UHFFFAOYSA-N cerium Chemical compound [Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce] ZMIGMASIKSOYAM-UHFFFAOYSA-N 0.000 description 1
- PZTQVMXMKVTIRC-UHFFFAOYSA-L chembl2028348 Chemical compound [Ca+2].[O-]S(=O)(=O)C1=CC(C)=CC=C1N=NC1=C(O)C(C([O-])=O)=CC2=CC=CC=C12 PZTQVMXMKVTIRC-UHFFFAOYSA-L 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
- JYWJULGYGOLCGW-UHFFFAOYSA-N chloromethyl chloroformate Chemical compound ClCOC(Cl)=O JYWJULGYGOLCGW-UHFFFAOYSA-N 0.000 description 1
- 229910000423 chromium oxide Inorganic materials 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 229910052570 clay Inorganic materials 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- KBLWLMPSVYBVDK-UHFFFAOYSA-N cyclohexyl prop-2-enoate Chemical compound C=CC(=O)OC1CCCCC1 KBLWLMPSVYBVDK-UHFFFAOYSA-N 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 150000001993 dienes Chemical class 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- YQGOJNYOYNNSMM-UHFFFAOYSA-N eosin Chemical compound [Na+].OC(=O)C1=CC=CC=C1C1=C2C=C(Br)C(=O)C(Br)=C2OC2=C(Br)C(O)=C(Br)C=C21 YQGOJNYOYNNSMM-UHFFFAOYSA-N 0.000 description 1
- 125000004185 ester group Chemical group 0.000 description 1
- 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
- PLYDMIIYRWUYBP-UHFFFAOYSA-N ethyl 4-[[2-chloro-4-[3-chloro-4-[(3-ethoxycarbonyl-5-oxo-1-phenyl-4h-pyrazol-4-yl)diazenyl]phenyl]phenyl]diazenyl]-5-oxo-1-phenyl-4h-pyrazole-3-carboxylate Chemical compound CCOC(=O)C1=NN(C=2C=CC=CC=2)C(=O)C1N=NC(C(=C1)Cl)=CC=C1C(C=C1Cl)=CC=C1N=NC(C(=N1)C(=O)OCC)C(=O)N1C1=CC=CC=C1 PLYDMIIYRWUYBP-UHFFFAOYSA-N 0.000 description 1
- STVZJERGLQHEKB-UHFFFAOYSA-N ethylene glycol dimethacrylate Substances CC(=C)C(=O)OCCOC(=O)C(C)=C STVZJERGLQHEKB-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
- 239000010419 fine particle Substances 0.000 description 1
- 239000001056 green pigment Substances 0.000 description 1
- 238000010438 heat treatment Methods 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
- LNCPIMCVTKXXOY-UHFFFAOYSA-N hexyl 2-methylprop-2-enoate Chemical compound CCCCCCOC(=O)C(C)=C LNCPIMCVTKXXOY-UHFFFAOYSA-N 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- NNGHIEIYUJKFQS-UHFFFAOYSA-L hydroxy(oxo)iron;zinc Chemical compound [Zn].O[Fe]=O.O[Fe]=O NNGHIEIYUJKFQS-UHFFFAOYSA-L 0.000 description 1
- 125000002768 hydroxyalkyl group Chemical group 0.000 description 1
- 235000019239 indanthrene blue RS Nutrition 0.000 description 1
- UHOKSCJSTAHBSO-UHFFFAOYSA-N indanthrone blue Chemical compound C1=CC=C2C(=O)C3=CC=C4NC5=C6C(=O)C7=CC=CC=C7C(=O)C6=CC=C5NC4=C3C(=O)C2=C1 UHOKSCJSTAHBSO-UHFFFAOYSA-N 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000002563 ionic surfactant Substances 0.000 description 1
- 230000005865 ionizing radiation Effects 0.000 description 1
- 229910052742 iron Inorganic materials 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
- CUSDLVIPMHDAFT-UHFFFAOYSA-N iron(3+);manganese(2+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[Mn+2].[Fe+3].[Fe+3] CUSDLVIPMHDAFT-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
- 239000006233 lamp black Substances 0.000 description 1
- 239000011133 lead Substances 0.000 description 1
- 235000010187 litholrubine BK Nutrition 0.000 description 1
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 description 1
- 239000001095 magnesium carbonate Substances 0.000 description 1
- 229910000021 magnesium carbonate Inorganic materials 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
- 230000005415 magnetization Effects 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
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 229920000609 methyl cellulose Polymers 0.000 description 1
- 239000001923 methylcellulose Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000006082 mold release agent Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910001000 nickel titanium Inorganic materials 0.000 description 1
- 125000000449 nitro group Chemical group [O-][N+](*)=O 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 239000002736 nonionic surfactant Substances 0.000 description 1
- WWZKQHOCKIZLMA-UHFFFAOYSA-N octanoic acid Chemical compound CCCCCCCC(O)=O WWZKQHOCKIZLMA-UHFFFAOYSA-N 0.000 description 1
- 239000001053 orange pigment 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
- 150000002978 peroxides Chemical class 0.000 description 1
- 239000012071 phase Substances 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
- 229920000767 polyaniline Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- HJWLCRVIBGQPNF-UHFFFAOYSA-N prop-2-enylbenzene Chemical compound C=CCC1=CC=CC=C1 HJWLCRVIBGQPNF-UHFFFAOYSA-N 0.000 description 1
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 239000001057 purple pigment Substances 0.000 description 1
- 150000003230 pyrimidines Chemical class 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
- 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
- 150000003839 salts Chemical class 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 229910052711 selenium Inorganic materials 0.000 description 1
- 239000011669 selenium Substances 0.000 description 1
- 229920002545 silicone oil Polymers 0.000 description 1
- 239000000344 soap Substances 0.000 description 1
- 239000012798 spherical particle Substances 0.000 description 1
- LXMSZDCAJNLERA-ZHYRCANASA-N spironolactone Chemical compound C([C@@H]1[C@]2(C)CC[C@@H]3[C@@]4(C)CCC(=O)C=C4C[C@H]([C@@H]13)SC(=O)C)C[C@@]21CCC(=O)O1 LXMSZDCAJNLERA-ZHYRCANASA-N 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000000454 talc Substances 0.000 description 1
- 229910052623 talc Inorganic materials 0.000 description 1
- CIHOLLKRGTVIJN-UHFFFAOYSA-N tert‐butyl hydroperoxide Chemical compound CC(C)(C)OO CIHOLLKRGTVIJN-UHFFFAOYSA-N 0.000 description 1
- 229920005992 thermoplastic resin Polymers 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 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 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
- UJMBCXLDXJUMFB-UHFFFAOYSA-K trisodium;5-oxo-1-(4-sulfonatophenyl)-4-[(4-sulfonatophenyl)diazenyl]-4h-pyrazole-3-carboxylate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)C1=NN(C=2C=CC(=CC=2)S([O-])(=O)=O)C(=O)C1N=NC1=CC=C(S([O-])(=O)=O)C=C1 UJMBCXLDXJUMFB-UHFFFAOYSA-K 0.000 description 1
- JEVGKYBUANQAKG-UHFFFAOYSA-N victoria blue R Chemical compound [Cl-].C12=CC=CC=C2C(=[NH+]CC)C=CC1=C(C=1C=CC(=CC=1)N(C)C)C1=CC=C(N(C)C)C=C1 JEVGKYBUANQAKG-UHFFFAOYSA-N 0.000 description 1
- 229920003169 water-soluble polymer Polymers 0.000 description 1
- 239000001993 wax Substances 0.000 description 1
- 239000012463 white pigment Substances 0.000 description 1
- 239000001052 yellow pigment Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
- 235000014692 zinc oxide Nutrition 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
Classifications
-
- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03G—ELECTROGRAPHY; ELECTROPHOTOGRAPHY; MAGNETOGRAPHY
- G03G9/00—Developers
- G03G9/08—Developers with toner particles
- G03G9/083—Magnetic toner particles
Landscapes
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Developing Agents For Electrophotography (AREA)
Abstract
Description
【発明の詳細な説明】
（産業上の利用分野）
本発明は、磁性トナーの製造方法に関し、より詳細には
弱磁性トナー及び非磁性トナー等の不良粒子の生成が防
止された磁性トナー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 magnetic toner, and more particularly to a method for producing magnetic toner in which generation of defective particles such as weakly magnetic toner and non-magnetic toner is prevented. Regarding the method.
（従来技術）
電子写真法を利用した複写機等においては、−般に光導
電性物質を利用し、種々の手段により怒光体上に電気的
潜像を形成し、次いで該潜像をトナーを用いて現像し、
必要に応じて紙等の転写材にトナー画像′を転写した後
、加熱、加圧或いは溶剤蒸気等によりトナー画像を定着
し、複写物を得るものである。 。(Prior Art) In copying machines and the like that utilize electrophotography, a photoconductive substance is generally used to form an electrical latent image on a photoreceptor by various means, and then the latent image is transferred to a toner. Develop using
After the toner image is transferred to a transfer material such as paper as necessary, the toner image is fixed by heating, pressure, solvent vapor, etc. to obtain a copy. .
上述するトナーを用いる現像方法としては、−般にキャ
リアと呼ばれる磁性粒子とトナーを混合して磁気ブラシ
を形成させ、潜像を摺擦して現像を行う二成分現像法や
、磁性体がトナー中に混入された磁性トナーによって磁
気ブラシを形成して現像を行う一成分現像法が広く用い
られている。Development methods using the above-mentioned toner include two-component development methods, in which magnetic particles generally called carriers and toner are mixed to form a magnetic brush, and the latent image is developed by rubbing it; A one-component development method is widely used in which development is performed by forming a magnetic brush using magnetic toner mixed therein.
しかしながら、二成分現像法においては、キャリアの劣
化やトナーとキャリアの混合比の変動によって現像特性
を悪化させるという欠点があり、一定の現像特性を得る
ためには種々の制御が必要となってくる。この反面、磁
性トナーを用いた一成分現像法は、キャリアを用いない
でよいので、キャリアとトナーの混合比の調整が不要で
あり、またキャリアとトナーを充分に混合するための攪
拌操作を特に必要としないことから、現像装置全体が簡
略でき、またコンパクトに構成できるという利点を有し
ている。However, the two-component development method has the disadvantage that development characteristics deteriorate due to deterioration of the carrier and fluctuations in the mixing ratio of toner and carrier, and various controls are required to obtain constant development characteristics. . On the other hand, the one-component development method using magnetic toner does not require the use of a carrier, so there is no need to adjust the mixing ratio of carrier and toner. Since this is not necessary, the entire developing device can be simplified and has the advantage that it can be constructed compactly.
このため、近年複写機の小型化、メンテナンスフリー化
等の要望から一成分現像法を利用した複写機等が多く使
用されるようになってきた。For this reason, in recent years, copying machines that utilize one-component development have come into widespread use due to the desire to make copying machines more compact and maintenance-free.
上記−成分現像法に使用される磁性トナーの製造方法と
しては、装置が簡略化でき、また操作も簡単であり効率
良く低コストでトナーが得られること、及び流動性及び
摩擦帯電性に優れ、現像スリーブ上に均一にトナー層が
形成できる球形のトナーが得られることから、懸濁重合
によるトナーの製造方法が多（使用されるようになって
きている。The method for manufacturing the magnetic toner used in the above-mentioned component development method is that the device is simple, the operation is easy, the toner can be obtained efficiently and at low cost, and it has excellent fluidity and triboelectric charging properties. Since a spherical toner that can form a uniform toner layer on a developing sleeve can be obtained, a method of manufacturing toner by suspension polymerization is increasingly being used.
この製造方法は定着樹脂を形成する重合性単量体、着色
剤、電荷制御剤、磁性粒子等の各種トナー構成材料と重
合開始剤の混合物を重合性組成物として、この重合性組
成物を水相中に投入して、懸濁攪拌してトナーサイズの
油滴粒子を生成し、生成された油的粒子を重合してトナ
ー粒子を一挙に製造するものである。This manufacturing method uses a mixture of various toner constituent materials such as polymerizable monomers forming the fixing resin, colorants, charge control agents, and magnetic particles, and a polymerization initiator as a polymerizable composition. The oil is added to the phase, suspended and stirred to produce toner-sized oil droplets, and the produced oily particles are polymerized to produce toner particles all at once.
そして、生成されるトナー粒子、特に磁性トナーにおい
ては各種構成材料は勿論のこと、磁性粒子が均−且つ一
様に分散していなければならず、トナー粒子中の磁性粒
子の含有量及び粒子内での磁性粒子の分散状態によって
、生成されるトナーの現像特性が異なったものとなり安
定した複写画像が得られなくなってしまう。In addition to various constituent materials, the generated toner particles, especially magnetic toner, must have magnetic particles evenly and uniformly dispersed, and the content of magnetic particles in the toner particles and the inside of the particles must be Depending on the state of dispersion of the magnetic particles, the developing characteristics of the produced toner will vary, making it impossible to obtain stable copied images.
例えば、磁性粒子を含まない非磁性トナー粒子が生成さ
れたり、或いｔよ磁性粒子の含有量が少なかったり、分
散不良によって生ずる弱磁性トナーが生成されたりする
と、現像器の現像スリーブにトナーを均一に塗布するこ
とが出来な（なり、画像にむらを生じる。また、過剰な
非磁性粒子及び弱磁性粒子によって現像スリーブを覆っ
てしまい、現像耐久性を悪くしてしまう。For example, if non-magnetic toner particles that do not contain magnetic particles are generated, or if the content of magnetic particles is less than t, or weakly magnetic toner is generated due to poor dispersion, the toner should not be placed in the developing sleeve of the developing device. It is not possible to apply the toner uniformly, causing unevenness in the image. Also, the developing sleeve is covered with excessive non-magnetic particles and weakly magnetic particles, resulting in poor development durability.
そこで、懸濁重合による磁性トナーの製造においては磁
性粒子と重合性単量体との親和性を高めるとともに、重
合組成物中での分散性を高めるために、従来より磁性粒
子を各磁力・ノブリング剤によって表面処理する等の磁
性粒子の表面改質が行われている。Therefore, in the production of magnetic toner by suspension polymerization, in order to increase the affinity between the magnetic particles and the polymerizable monomer, as well as to increase the dispersibility in the polymer composition, conventionally, magnetic particles are Surface modification of magnetic particles, such as surface treatment with agents, is being carried out.
（発明が解決しようとする問題点）
しかしながら、マグネタイトをはじめとする磁性粒子は
真比重が大きく、磁性粒子の表面改質を行っても、水中
で重合性組成物の懸濁造粒時及び重合反応時に油滴粒子
内から磁性粒子が遊離し、磁性粒子の含有量が少ない弱
磁性トナー粒子或いは非磁性トナー粒子の生成を防止す
ることができないのが現状である。(Problems to be Solved by the Invention) However, magnetic particles such as magnetite have a large true specific gravity, and even if the surface of the magnetic particles is modified, it will not be possible to carry out suspension granulation and polymerization of a polymerizable composition in water. At present, magnetic particles are liberated from within the oil droplet particles during the reaction, and it is currently impossible to prevent the generation of weakly magnetic toner particles or non-magnetic toner particles with a small content of magnetic particles.
また、一般に磁性トナーにおいては、磁性粒子の充填率
は２０乃至８０％と高く油滴粒子全体の比重も大きなも
のとなり、重合反応中に油滴粒子の液滴が沈澱し１．凝
集体を形成してしまい収率を低下させてしまう。Furthermore, in general, in magnetic toner, the filling rate of magnetic particles is as high as 20 to 80%, and the specific gravity of the entire oil droplet particles is also large, and the droplets of the oil droplet particles settle during the polymerization reaction. Aggregates are formed and the yield is reduced.
本発明は上述する従来技術の問題点を解決するために成
されたものであり、本発明の目的は、油滴粒子内からの
磁性粒子の脱落を防止し、磁性粒子の含有量が均一で、
しかも−様に分散した磁性トナーが得られる製造方法を
提供することにある。The present invention has been made in order to solve the problems of the prior art described above, and an object of the present invention is to prevent magnetic particles from falling out of oil droplets and to maintain a uniform content of magnetic particles. ,
Moreover, it is an object of the present invention to provide a manufacturing method capable of obtaining a magnetic toner dispersed in a -like manner.
更に、本発明の他の目的は、多数枚複写においても画像
むら等を発生させることのない磁性トナーの製造方法を
提供することにある。更に、本発明の他の目的は、収率
良く磁性トナーを製造する方法を提供することにある。Another object of the present invention is to provide a method for producing magnetic toner that does not cause image unevenness even when copying a large number of sheets. Furthermore, another object of the present invention is to provide a method for producing magnetic toner with good yield.
（問題点を解決する為の手段）
懸濁重合を用いた磁性トナーの製造方法において、重合
系に磁界を作用させながら重合反応を行うことにより、
従来からの問題点が解決され、本発明の目的が達成され
る。(Means for solving the problem) In a method for manufacturing magnetic toner using suspension polymerization, by performing a polymerization reaction while applying a magnetic field to the polymerization system,
The conventional problems are solved and the objects of the present invention are achieved.
（作用）
本発明者は懸濁造粒して油滴粒子を生成する工程及び重
合反応を行う工程中に、重合系に磁場を作用させること
により、磁力作用によって油滴粒子内の磁性粒子と重合
性単量体及び水性媒体との比重差によって生ずる油滴粒
子からの磁性粒子の脱落が防止でき、更に油的粒子内に
安定に存在させて重合反応が行え、均一磁性を有するト
ナーが収率良く製造できる方法を見出したのである。(Function) The present inventor applied a magnetic field to the polymerization system during the process of generating oil droplets by suspension granulation and the process of performing a polymerization reaction, thereby causing the magnetic particles in the oil droplets to The magnetic particles can be prevented from falling off from the oil droplet particles due to the difference in specific gravity between the polymerizable monomer and the aqueous medium, and furthermore, the magnetic particles can be stably present in the oil particles and the polymerization reaction can be carried out, producing toner with uniform magnetic properties. They discovered a method that allows for efficient production.
以下、第１図に示す重合装置の一例により本発明を説明
する。第１図に示されるように重合性単量体、着色剤、
電荷制御剤、磁性粒子及び重合開始剤等の混合物である
重合性組成物を充分に分散させた後、試料投入口２より
、分散安定剤が溶解乃至分散された水相３中に投入し、
不活性ガス導入口４よりＮ！等の不活性ガスを導入しつ
つ、攪拌器５により攪拌操作を行う。そして重合性組成
物の投入と同時か或いは、撹拌操作と平行して、重合装
置上部に配置された磁界発生手段１によって、一定の磁
界をかけながら攪拌操作を続行して、トナーサイズの油
的粒子を生成する。そして、懸濁造粒して得られた油的
粒子が分散した水相に更に磁界を作用させながら、重合
槽８の周囲を囲む温水ジャケット中６に温水を導入して
重合槽８を昇温し、重合反応を進行させて重合が完結し
た後に、重合体粒子を回収し、乾燥してトナーとする。The present invention will be explained below using an example of a polymerization apparatus shown in FIG. As shown in Figure 1, polymerizable monomers, colorants,
After sufficiently dispersing the polymerizable composition, which is a mixture of a charge control agent, magnetic particles, a polymerization initiator, etc., it is introduced from the sample input port 2 into the aqueous phase 3 in which the dispersion stabilizer is dissolved or dispersed,
N from inert gas inlet port 4! A stirring operation is performed using the stirrer 5 while introducing an inert gas such as. Then, at the same time as the addition of the polymerizable composition or in parallel with the stirring operation, the stirring operation is continued while applying a constant magnetic field by the magnetic field generating means 1 disposed at the top of the polymerization apparatus, so that the oil of the toner size is Generate particles. Then, while applying a magnetic field to the aqueous phase in which the oil particles obtained by suspension granulation are dispersed, hot water is introduced into the hot water jacket 6 surrounding the polymerization tank 8 to raise the temperature of the polymerization tank 8. After the polymerization reaction is allowed to proceed and the polymerization is completed, the polymer particles are collected and dried to form a toner.
（図中７は冷却官である。） 以下、更に詳細に説明する。(7 in the figure is the cooling officer.) This will be explained in more detail below.
本発明に使用される磁界発生手段としては、静磁界を発
生する永久磁石、動磁界を発生する電磁石等の一般に使
用される磁界を発生するものなら何れも使用することが
できる。As the magnetic field generating means used in the present invention, any commonly used magnetic field generating means can be used, such as a permanent magnet that generates a static magnetic field and an electromagnet that generates a dynamic magnetic field.
そして、上記説明した図においては磁界発生手段を装置
の上方に設けたが、重合工程において重合反応装置の上
方、下方、側方のうちの少なくとも一方に磁界発生手段
を設けることができ、一定磁界を継続して作用させるか
、或いは断続的に作用させてもよく、また、磁界の強さ
を変化させたり、磁界の橿を変えながら作用させてもよ
く、攪拌速度及び磁性粒子の比重及び磁化力によって適
宜使用条件が設定できる。そして、上記操作は永久磁石
を回転させて使用させたり、電磁石の通電操作等によっ
て行うことができる。In the diagrams explained above, the magnetic field generating means is provided above the apparatus, but in the polymerization process, the magnetic field generating means can be provided above, below, or at least on the sides of the polymerization reaction apparatus, and a constant magnetic field can be provided. The magnetic field may be applied continuously or intermittently, or may be applied while changing the strength of the magnetic field or the beam of the magnetic field, and the stirring speed, the specific gravity of the magnetic particles, and the magnetization Conditions of use can be set as appropriate depending on the power. The above operation can be performed by rotating a permanent magnet or by energizing an electromagnet.
上記磁界発生手段によって作用させる磁界の強さとして
は、一般的に重合系の中心において１乃至１０００Ｇ（
ガウス）、特に１０乃至２００Ｇ（ガウス）程度が必要
である。また、攪拌器による撹拌の速度としては、造粒
時においては、一般的に１乃至１１０００ｒｐ、特に１
０乃至２００ｒｐｍが好ましい、また、重合時には一般
に２０乃至５００ｒｐｍ、特に５０乃至２００ｒｐｍが
好ましい。The strength of the magnetic field applied by the magnetic field generating means is generally 1 to 1000 G (
(Gauss), especially about 10 to 200 G (Gauss). In addition, the speed of stirring by the stirrer is generally 1 to 11,000 rp, especially 1 to 11,000 rpm during granulation.
0 to 200 rpm is preferred, and generally 20 to 500 rpm, especially 50 to 200 rpm during polymerization.
本発明において使用される重合性組成物を構成する重合
性単量体としては、定着性及び帯電性とを有する熱可塑
性樹脂を形成し得るものであり、ビニル芳香族単量体、
アクリル単量体、ビニルエステル単量体、ビニルエーテ
ル系単量体、ジオレフィン系単量体、モノオレフィン系
単量体等である。The polymerizable monomers constituting the polymerizable composition used in the present invention are those capable of forming a thermoplastic resin having fixing properties and charging properties, and include vinyl aromatic monomers,
These include acrylic monomers, vinyl ester monomers, vinyl ether monomers, diolefin monomers, monoolefin monomers, and the like.
ビニル芳香族単量体としては
式、
式中、Ｒ１は水素原子、低級アルキル基又はハロゲン原
子であり、Ｒｔは水素原子、低級ア）ｌｉ−Ｊｒ）Ｌ４
、ハロゲン原子、アルコキシ基、ニトロ基、或いはビニ
ル基でアル、
のビニル芳香族炭化水素、例えばスチレン、α−メチル
スチレン、ビニルトルエン、α−クロロスチレン、０−
１ｍ−１ｐ−クロロスチレン、ｐ−エチルスチレン、ジ
ビニルベンゼンの単独または２種以上の組み合わせを挙
５ｉｔｔ系でき、更に前述した他の単量体としては以下
のものを挙げることができる。The vinyl aromatic monomer has the following formula: In the formula, R1 is a hydrogen atom, a lower alkyl group, or a halogen atom, and Rt is a hydrogen atom, lower a)li-Jr)L4
, a halogen atom, an alkoxy group, a nitro group, or a vinyl group, such as styrene, α-methylstyrene, vinyltoluene, α-chlorostyrene, 0-
1m-1p-chlorostyrene, p-ethylstyrene, and divinylbenzene may be used alone or in combination of two or more thereof, and other monomers mentioned above may include the following.
式、
式中、Ｒ３は水素原子又は低級アルキル基Ｒ４は水素原
子、炭素数１２迄の炭化水素基、ヒドロキシルアルキル
基、或いはビニルエステル基である、
のアクリル系単量体、例えばアクリル酸メチル、アクリ
ル酸エチル、アクリル酸ブチル、アクリル酸−２−エチ
ルヘキシル、アクリル酸シクロヘキシル、アクリル酸フ
ェニル、メタクリル酸メチル、メタクリル酸ヘキシル、
メタクリル酸−２−エチルヘキシル、β−ヒドロキシア
クリル酸エチル、Ｔ−ヒドロキシアクリル酸プロピル、
σ−ヒドロキシアクリル酸ブチル、β−ヒドロキシメタ
クリル酸エチル、エチレングリコールジメタクリル酸エ
ステル、テトラエチレングリコールジメタクリル酸エス
テル等。Acrylic monomers, such as methyl acrylate, of the formula, where R3 is a hydrogen atom or a lower alkyl group R4 is a hydrogen atom, a hydrocarbon group having up to 12 carbon atoms, a hydroxyalkyl group, or a vinyl ester group; Ethyl acrylate, butyl acrylate, 2-ethylhexyl acrylate, cyclohexyl acrylate, phenyl acrylate, methyl methacrylate, hexyl methacrylate,
2-ethylhexyl methacrylate, ethyl β-hydroxyacrylate, propyl T-hydroxyacrylate,
σ-hydroxybutyl acrylate, β-hydroxyethyl methacrylate, ethylene glycol dimethacrylate, tetraethylene glycol dimethacrylate, etc.
式、
Ｏ
式中、Ｒ３は水素原子又は低級アルキル基である、
のビニルエステル、例えばギ酸ビニル、酢酸ビニル、プ
ロピオン酸ビニル等。Vinyl esters of the formula, O in which R3 is a hydrogen atom or a lower alkyl group, such as vinyl formate, vinyl acetate, vinyl propionate, etc.
式、
式中、Ｒｈは炭素数１２迄の１価炭化水素基である、
のビニルエーテル、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、ビニルシクロへキサシル
エーテル等。Vinyl ethers of the formula, wherein Rh is a monovalent hydrocarbon group having up to 12 carbon atoms, such as vinyl-n-butyl ether, vinyl phenyl ether, vinyl cyclohexacyl ether, etc.
式、
式中、Ｒ？ 、Ｒｓ 、Ｒｑの各々は水素原子、低級ア
ルキル基又はハロゲン原子である、のジオレフィン類、
特にブタジェン、イソプレン、クロロブレン類。Formula, in the formula, R? , Rs and Rq are each a hydrogen atom, a lower alkyl group or a halogen atom,
Especially butadiene, isoprene, and chloroprenes.
式、
式中、Ｒ１゜、Ｒ１１の各々は水素原子又は低級アルキ
ル基である、
のモノオレフィン類、特にエチレン、プロピレン、イソ
ブチレン、ブテン−１、ペンテン−１１４−メチルペン
テン−１等。Monoolefins of the formula, in which each of R1° and R11 is a hydrogen atom or a lower alkyl group, particularly ethylene, propylene, isobutylene, butene-1, pentene-114-methylpentene-1, etc.
好適な単量体は、スチレン系単量体、アクリル系単量体
等である。Suitable monomers include styrene monomers and acrylic monomers.
本発明に使用される着色剤としては、以下に記す種々の
顔料や染料（以下単に着色顔料と呼ぶ）が前記単量体に
含有させて使用できる。As the coloring agent used in the present invention, various pigments and dyes (hereinafter simply referred to as colored pigments) described below can be used by incorporating them into the monomer.
黒色顔料
カーボンブラック、アセチレンブラック、ランプブラッ
ク、アニリンブラック。Black pigments carbon black, acetylene black, lamp black, aniline black.
黄色顔料
黄鉛、亜鉛黄、カドミウムイエロー、黄色酸化鉄、ミネ
ラルファーストイエロー、ニッケルチタンイエロー、ネ
ーブルスイエロー、ナフトールイエローＳ１ハンザイエ
ロー１０Ｇ、ベンジジンイエローＧ１キノリンイエロー
レーキ、パーマネンエローＮＣＧ、タートラジンレーキ
。Yellow pigments yellow lead, zinc yellow, cadmium yellow, yellow iron oxide, mineral first yellow, nickel titanium yellow, navels yellow, naphthol yellow S1 Hansa yellow 10G, benzidine yellow G1 quinoline yellow lake, permanent yellow NCG, tartrazine lake.
橙色顔料
赤口黄鉛、モリブテンオレンジ、パーマネントオレンジ
ＧＴＲ，ピラゾロンオレンジ、パルカンオレンジ、イン
ダンスレンブリリアントオレンジＲＫ、ベンジジンオレ
ンジＧ１インダンスレンブリリアントオレンジＧＫ。Orange pigment red yellow lead, molybdenum orange, permanent orange GTR, pyrazolone orange, palkan orange, indanthrene brilliant orange RK, benzidine orange G1 indanthrene brilliant orange GK.
赤色顔料
ベンガラ、カドミュウムレッド、鉛丹、硫化水銀カドミ
ウム、パーマネントオレンジ４Ｒ，リソールレッド、ピ
ラゾロンレッド、ウオッチングレッドカルシウム塩、レ
ーキレッドＤ、ブリリアンドカーミン６Ｂ、エオシンレ
ーキ、ローダミンレーキＢ、アリザリンレーキ、ブリリ
アントカーミン３Ｂ。Red pigment Red pigment Red Garla, Cadmium Red, Red Lead, Mercury Cadmium Sulfide, Permanent Orange 4R, Lysole Red, Pyrazolone Red, Watching Red Calcium Salt, Lake Red D, Brilliant Carmine 6B, Eosin Lake, Rhodamine Lake B, Alizarin Lake , Brilliant Carmine 3B.
紫色顔料
マンガン紫、ファーストバイオレットＢ１メチルバイオ
レットレーキ。Purple pigment Manganese Purple, First Violet B1 Methyl Violet Lake.
青色顔料
紺青、コバルトブルー、アルカリブルーレーキ、ビクト
リアブルーレーキ、フタロシアニンブルー、無金属フタ
ロシアニンブルー、フタロシアニンブル一部分塩素化物
、ファーストスカイブルー、インダンスレンブル−ＢＣ
。Blue pigments navy blue, cobalt blue, alkali blue lake, Victoria blue lake, phthalocyanine blue, metal-free phthalocyanine blue, phthalocyanine blue partially chlorinated product, first sky blue, indanthremble-BC
.
緑色顔料
クロムグリーン、酸化クロム、ピグメントグリーンＢ１
マラカイトグリーンレーキ、ファナルイエローグリーン
Ｇ。Green pigment chrome green, chromium oxide, pigment green B1
Malachite Green Lake, Fanal Yellow Green G.
白色顔料 亜鉛華、酸化チタン、アンチモン白、硫化亜鉛。white pigment Zinc white, titanium oxide, antimony white, zinc sulfide.
体質顔料
パライト粉、炭酸バリウム、クレー、シリカ、ホワイト
カーボン、タルク、アルミホワイト。Extender pigments Palite powder, barium carbonate, clay, silica, white carbon, talc, aluminum white.
等が挙げられる。etc.
前記単量体と着色剤との量比はかなり大幅に変化させ得
るが、−船釣に言って、単量体１００重量部当たり１乃
至２０重量部、特に３乃至１０重量部が好適に用いるこ
とができる。The ratio of the monomers to the colorant can vary considerably, but - for boat fishing, 1 to 20 parts by weight, especially 3 to 10 parts by weight per 100 parts by weight of monomer are preferably used. be able to.
本発明に使用される磁性粒子としては、例えば四三酸化
鉄（Ｆｅｓ０４） 、三二酸化鉄（１−Ｐｅ＊０＊ ）
、酸化鉄亜鉛（ＺｎＦｅｔＯｎ） 、酸化鉄イツトリウ
ム（ＹｚＦｅｓＯ＋ｔ）、酸化カドミウム（Ｇｄ３ＦＥ
ｌｓＯ＋ｔ） 、酸化鉄１ｉ１（ＣｕＦｅｚＯａ）、酸
化鉄錯（ＰｂＦｅｔｔＯ＋ｗ） 、酸化鉄ネオジウム（
ＮｄＦｅＯ＊）、酸化鉄バリウム（ＢａＦｅ ｌｔＯｔ
９）、酸化鉄マグネシウム（ＭｇＦｅｔＯｎ） 、酸化
鉄マンガン（ＭｎＰｅｔ０４） 、酸化鉄ランタン（Ｌ
ａＦｅＯｓ）、鉄粉（Ｆｅ）、コバルト粉 （ＣＯ）、
ニッケル粉（Ｎｉ）等の公知の磁性材料の微粒子の任意
のものを一種或いは二種以上を混合して用いることがで
きる。Examples of magnetic particles used in the present invention include triiron tetroxide (Fes04) and iron sesquioxide (1-Pe*0*).
, zinc iron oxide (ZnFetOn), yttrium iron oxide (YzFesO+t), cadmium oxide (Gd3FE)
lsO+t), iron oxide 1i1 (CuFezOa), iron oxide complex (PbFettO+w), iron neodymium oxide (
NdFeO*), barium iron oxide (BaFe ltOt)
9), Magnesium iron oxide (MgFetOn), Manganese iron oxide (MnPet04), Lanthanum iron oxide (L
aFeOs), iron powder (Fe), cobalt powder (CO),
Any known fine particles of magnetic material such as nickel powder (Ni) can be used alone or in combination of two or more.
上記磁性粒子は前述した単量体１００重量部当たり２０
乃至８０重量部、特に３０乃至７０重量部が好ましく用
いられる。The above magnetic particles are 20% by weight per 100 parts by weight of the above-mentioned monomer.
80 to 80 parts by weight, particularly 30 to 70 parts by weight, is preferably used.
また、本発明に使用される重合開始剤としては、アゾビ
スイソブチロニトリル等のアゾ化合物や、クメンヒドロ
ペルオキシド、ｔ−ブチルヒドロペルオキシド、ジクミ
ルペルオキシド、ジーＬ−ブチルペルオキシド、過酸化
ベンゾイル、過酸化ラウロイル等の過酸化物等の油溶性
の開始剤が使用される。これら重合開始剤は重合性単量
体１００重量部当たり０．１乃至１０重量部が好ましく
使用される。Further, as the polymerization initiator used in the present invention, azo compounds such as azobisisobutyronitrile, cumene hydroperoxide, t-butyl hydroperoxide, dicumyl peroxide, di-L-butyl peroxide, benzoyl peroxide, Oil-soluble initiators such as peroxides such as lauroyl peroxide are used. These polymerization initiators are preferably used in an amount of 0.1 to 10 parts by weight per 100 parts by weight of the polymerizable monomer.
また、帯電立ち上がり、帯電安定性及び環境安定性等の
目的で公知の電荷制御剤を重合反応に影響を与えない程
度で使用することができる。Further, for the purpose of charging rise, charging stability, environmental stability, etc., a known charge control agent can be used to the extent that it does not affect the polymerization reaction.
これら電荷制御剤としては、ニグロシン染料、オイルブ
ラック、スピロンブラック等の油溶性染料や、ナフテン
酸、サリチル酸、オクチル酸、高級脂肪酸、樹脂酸のマ
ンガン、鉄、コバルト、鉛、亜鉛、セリウム、カルシウ
ム、ニッケル等の金属塩である金属石鹸等或いは含金属
アゾ染料、ピリミジン化合物、アルキルサリチル酸金属
キレート等を一般的に前記重合性単量体１００重量部当
たり０． １乃至１０重量部、特にｌ乃至５重量部添加
することができる。These charge control agents include oil-soluble dyes such as nigrosine dye, oil black, and spirone black, naphthenic acid, salicylic acid, octylic acid, higher fatty acids, and resin acids such as manganese, iron, cobalt, lead, zinc, cerium, and calcium. , metal soaps such as metal salts such as nickel, metal-containing azo dyes, pyrimidine compounds, alkyl salicylic acid metal chelates, etc. are generally added in an amount of 0.00 parts per 100 parts by weight of the polymerizable monomer. 1 to 10 parts by weight, especially 1 to 5 parts by weight can be added.
また、オフセット防止剤として低分子量ポリエチレン、
低分子量ポリプロピレン、各種ワックス、シリコーン油
等の離型剤を含有させることもできる。In addition, low molecular weight polyethylene is used as an anti-offset agent.
It is also possible to contain a mold release agent such as low molecular weight polypropylene, various waxes, and silicone oil.
これら、オフセット防止剤は重合性単量体１００重量部
当たり０．１乃至１０重量部、特に１乃至５重量部が好
ましく使用される。These offset inhibitors are preferably used in an amount of 0.1 to 10 parts by weight, particularly 1 to 5 parts by weight, per 100 parts by weight of the polymerizable monomer.
また、上述した重合性単量体及び各種添加剤からなる重
合性組成物を水媒体中に懸濁して、油滴粒子として安定
化させる分散安定剤としては、ポリビニルアルコール、
メチルセルロース等の水溶性高分子やノニオン系或いは
イオン系の界面活性剤、難水溶性無機塩微粉末等が使用
される。特に、粒子の均一安定性、及び後処理の点から
難水溶性無機塩微粉末が好ましく使用される。これら難
水溶性無機塩微粉末としては硫酸カルシウム、リン酸カ
ルシウム、炭酸マグネシウム、炭酸バリウム、炭酸カル
シウム、水酸化アルミニウム等が使用される。Further, as a dispersion stabilizer for suspending the polymerizable composition consisting of the above-mentioned polymerizable monomer and various additives in an aqueous medium and stabilizing it as oil droplet particles, polyvinyl alcohol, polyvinyl alcohol,
Water-soluble polymers such as methylcellulose, nonionic or ionic surfactants, and slightly water-soluble inorganic salt fine powders are used. In particular, poorly water-soluble inorganic salt fine powder is preferably used from the viewpoint of uniform stability of particles and post-treatment. As these poorly water-soluble inorganic salt fine powders, calcium sulfate, calcium phosphate, magnesium carbonate, barium carbonate, calcium carbonate, aluminum hydroxide, etc. are used.
上記分散安定剤は氷島たり０．１乃至５０重量％、特に
１乃至１０重量％の量で加えるとよい。The above-mentioned dispersion stabilizer is preferably added in an amount of 0.1 to 50% by weight, particularly 1 to 10% by weight per ice island.
また、重合反応はＴ−線、加速電子線のようなイオン化
放射線や各種増感剤との組み合わせによっても行うこと
ができる。Further, the polymerization reaction can also be carried out using ionizing radiation such as T-rays or accelerated electron beams, or in combination with various sensitizers.
重合開始温度及び時間は、公知のそれでよく、一般に４
０乃至１００℃の温度で１時間乃至５０時間の重合で充
分である。The polymerization initiation temperature and time may be any known ones, and are generally 4.
Polymerization for 1 to 50 hours at a temperature of 0 to 100°C is sufficient.
懸濁油滴の粒子サイズは、５μｍ乃至３０μｍ、特に８
μｍ乃至２０μｍに調節するのが適当である。The particle size of the suspended oil droplets is between 5 μm and 30 μm, especially 8 μm.
It is appropriate to adjust the thickness to between μm and 20 μm.
そして、本発明においては、前述した磁界発生手段によ
って重合系中に磁界を作用させて、油滴粒子内の磁性粒
子に対して、攪拌による遠心力及び磁性粒子の比重によ
る沈降力を抑制して重合反応を行い完結させる。In the present invention, a magnetic field is applied to the polymerization system by the above-mentioned magnetic field generating means to suppress the centrifugal force caused by stirring and the sedimentation force caused by the specific gravity of the magnetic particles on the magnetic particles within the oil droplet particles. The polymerization reaction is carried out and completed.
反応後の重合生成物は前述した粒度範囲で球形の粒状物
の形で得られ、この生成粒子を濾過し、必要により水ま
たは適当な溶剤で洗浄し、乾燥して、トナー粒子とする
。The polymerized product after the reaction is obtained in the form of spherical particles in the above-mentioned particle size range, and the resulting particles are filtered, washed if necessary with water or a suitable solvent, and dried to form toner particles.
このトナー粒子には、必要により、カーボンブラック、
疎水性シリカ等をまぶして、最終トナーとする。The toner particles may contain carbon black, if necessary.
Sprinkle hydrophobic silica etc. to make the final toner.
以下に、実施例及び比較例により本発明を更に詳細に説
明する。The present invention will be explained in more detail below using Examples and Comparative Examples.
（合成例１）
マグネタイト ５０重量部スチレンモ
ノマー ３０重量部ｎ−ブチルメタクリレ
ート ２０重量部電荷制御剤（ボントロン５−３４
、
オリエント化学社製）
１重量部
ジビニルベンゼン １ｍｆｆ１部をボー
ルミルにて充分に分散した後、重合開始剤としてＡＩＢ
Ｎを１重量部加え、２％のＰＶＡ水溶液４００重量部中
に投入し、反応槽の上部に永久磁石を設け、反応槽の中
心での磁界の強さが１００Ｇに成るように調整して、Ｔ
Ｋホモミキサーによて５０００ｒｐｍｌＯ分間懸濁分散
させ平均粒径が１５μｍの油滴粒子を生成した。(Synthesis Example 1) Magnetite 50 parts by weight Styrene monomer 30 parts by weight n-butyl methacrylate 20 parts by weight Charge control agent (Bontron 5-34
(manufactured by Orient Chemical Co., Ltd.) 1 part by weight divinylbenzene 1 mff 1 part was sufficiently dispersed in a ball mill, and then AIB was added as a polymerization initiator.
Add 1 part by weight of N and pour into 400 parts by weight of a 2% PVA aqueous solution, install a permanent magnet at the top of the reaction tank, and adjust the magnetic field strength at the center of the reaction tank to 100G. T
The mixture was suspended and dispersed using a K homomixer for 5,000 rpm and 10 minutes to produce oil droplets with an average particle size of 15 μm.
そして、更に磁界の強さを５０Ｇに設定し、窒素雰囲気
下８０°Ｃに昇温しで１０時間重合して反応を完結させ
た。Then, the strength of the magnetic field was further set to 50 G, the temperature was raised to 80° C. under a nitrogen atmosphere, and the reaction was completed by polymerizing for 10 hours.
得られたトナー粒子をデカンテーシヨン、濾過、熱水処
理、乾燥して本発明の磁性トナーを得た。The obtained toner particles were decanted, filtered, treated with hot water, and dried to obtain a magnetic toner of the present invention.
このトナーの粒度分布をコールタ−カウンターを用いて
測定したところ、体積平均径は１５．３μｍで５μｍ以
下の微粉トナーは０．２％であった。When the particle size distribution of this toner was measured using a Coulter counter, the volume average diameter was 15.3 .mu.m, and the amount of fine powder toner of 5 .mu.m or less was 0.2%.
得られたトナーを用い、感光体にセレンドラムを用い、
非磁性部材を介してマグネットを内蔵した現像スリーブ
（外径３３ｍｍ）上の磁場の強さを８００ガウスとし、
穂切り板とスリーブの間隔を０．３ｍｍとした一成分現
像装置を搭載したＤＣ−１１１Ｃ（三田工業社製）改造
機において画像形成したところ、カブリのない鮮明な画
像が得られた、また２万枚に及ぶ耐刷試験においても画
像の変動は無（、スリーブへの非磁性トナー及び弱磁性
トナーの付着も無かった。Using the obtained toner and using a selenium drum as a photoreceptor,
The strength of the magnetic field on the developing sleeve (outer diameter 33 mm) containing a magnet via a non-magnetic member was set to 800 Gauss,
When images were formed using a modified DC-111C (manufactured by Sanda Kogyo Co., Ltd.) equipped with a one-component developing device with a spacing of 0.3 mm between the cutting board and the sleeve, clear images without fogging were obtained. Even in a printing durability test of 10,000 sheets, there was no change in the image (and there was no adhesion of non-magnetic toner or weakly magnetic toner to the sleeve).
（比較例１）
実施例において磁界を作用させず、他は同様にして重合
反応を行い、磁性トナーを得た。(Comparative Example 1) A polymerization reaction was carried out in the same manner as in Example except that no magnetic field was applied, and a magnetic toner was obtained.
得られたトナーを実施例と同様にして画像形成したとこ
ろカブリが認められた。また、２万枚の耐刷試験おいて
は、複写枚数の増大とともに画像濃度が低下し、現像器
内においてはスリーブ上に不良トナー粒子が付着し、消
費されずに残留していた。When an image was formed using the obtained toner in the same manner as in the example, fogging was observed. In addition, in a 20,000-sheet printing test, the image density decreased as the number of copies increased, and defective toner particles adhered to the sleeve in the developing device and remained unconsumed.
（発明の効果）
本発明によれば、懸濁重合による磁性トナーの製造にお
いて、重合性組成物の造粒時及び造粒して得られた油的
粒子の重合時に磁性粒子が油的粒子内から脱落すること
なく、磁性粒子が均一に分散した状態で重合反応を完結
することができる。(Effects of the Invention) According to the present invention, in the production of magnetic toner by suspension polymerization, magnetic particles are contained within the oily particles during granulation of the polymerizable composition and during polymerization of the oily particles obtained by granulation. The polymerization reaction can be completed in a state where the magnetic particles are uniformly dispersed without falling off.
そして、得られるトナーは非磁性トナー粒子及び弱磁性
トナー粒子を少なくすることができ、該トナーによって
得られる画像はカブリがなく鮮明な画像が得られ、多数
枚の連続複写においても安定した画像が得られる。The resulting toner can reduce the amount of non-magnetic toner particles and weakly magnetic toner particles, and the images obtained with this toner are clear and fog-free, and are stable even when continuously copying a large number of sheets. can get.
第１図は、本発明に使用される重合装置の一例をしめず
概略図である。
１・・・磁界発生手段 ２・・・試料投入口５・・・攪
拌器 ８・・・重合槽FIG. 1 is a schematic diagram of an example of a polymerization apparatus used in the present invention. 1... Magnetic field generating means 2... Sample inlet 5... Stirrer 8... Polymerization tank
Claims (1)
徴とする磁性トナーの製造方法。[Scope of Claims] A method for producing a magnetic toner using suspension polymerization, characterized in that the polymerization reaction is carried out while applying a magnetic field to the polymerization system.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63108085A JPH01277254A (en) | 1988-04-28 | 1988-04-28 | Manufacture of magnetic toner |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63108085A JPH01277254A (en) | 1988-04-28 | 1988-04-28 | Manufacture of magnetic toner |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH01277254A true JPH01277254A (en) | 1989-11-07 |
Family
ID=14475495
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP63108085A Pending JPH01277254A (en) | 1988-04-28 | 1988-04-28 | Manufacture of magnetic toner |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH01277254A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0858007A1 (en) * | 1997-02-10 | 1998-08-12 | Canon Kabushiki Kaisha | Process for producing toner for developing electrostatic images |
-
1988
- 1988-04-28 JP JP63108085A patent/JPH01277254A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0858007A1 (en) * | 1997-02-10 | 1998-08-12 | Canon Kabushiki Kaisha | Process for producing toner for developing electrostatic images |
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