JPH01224755A - Silver halide color photosensitive material - Google Patents
Silver halide color photosensitive materialInfo
- Publication number
- JPH01224755A JPH01224755A JP5128688A JP5128688A JPH01224755A JP H01224755 A JPH01224755 A JP H01224755A JP 5128688 A JP5128688 A JP 5128688A JP 5128688 A JP5128688 A JP 5128688A JP H01224755 A JPH01224755 A JP H01224755A
- Authority
- JP
- Japan
- Prior art keywords
- layer
- group
- silver
- silver halide
- sensitivity
- 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
- -1 Silver halide Chemical class 0.000 title claims abstract description 105
- 239000000463 material Substances 0.000 title claims abstract description 77
- 229910052709 silver Inorganic materials 0.000 title claims abstract description 74
- 239000004332 silver Substances 0.000 title claims abstract description 74
- 239000000839 emulsion Substances 0.000 claims abstract description 108
- 230000035945 sensitivity Effects 0.000 claims abstract description 56
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 20
- 238000004061 bleaching Methods 0.000 claims abstract description 14
- 150000001875 compounds Chemical group 0.000 claims description 46
- 125000003118 aryl group Chemical group 0.000 claims description 12
- 150000001412 amines Chemical class 0.000 claims description 2
- 238000012545 processing Methods 0.000 abstract description 23
- 230000001590 oxidative effect Effects 0.000 abstract description 3
- 239000007800 oxidant agent Substances 0.000 abstract 2
- 239000010410 layer Substances 0.000 description 140
- 238000000034 method Methods 0.000 description 55
- 239000000975 dye Substances 0.000 description 54
- JKFYKCYQEWQPTM-UHFFFAOYSA-N 2-azaniumyl-2-(4-fluorophenyl)acetate Chemical compound OC(=O)C(N)C1=CC=C(F)C=C1 JKFYKCYQEWQPTM-UHFFFAOYSA-N 0.000 description 38
- 229910021612 Silver iodide Inorganic materials 0.000 description 38
- 229940045105 silver iodide Drugs 0.000 description 38
- 108010010803 Gelatin Proteins 0.000 description 36
- 229920000159 gelatin Polymers 0.000 description 36
- 239000008273 gelatin Substances 0.000 description 36
- 235000019322 gelatine Nutrition 0.000 description 36
- 235000011852 gelatine desserts Nutrition 0.000 description 36
- 230000001235 sensitizing effect Effects 0.000 description 33
- ZUNKMNLKJXRCDM-UHFFFAOYSA-N silver bromoiodide Chemical compound [Ag].IBr ZUNKMNLKJXRCDM-UHFFFAOYSA-N 0.000 description 27
- 239000000243 solution Substances 0.000 description 27
- 239000006185 dispersion Substances 0.000 description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 25
- 125000004432 carbon atom Chemical group C* 0.000 description 24
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 21
- 239000002245 particle Substances 0.000 description 19
- 239000002253 acid Substances 0.000 description 17
- 150000003839 salts Chemical class 0.000 description 17
- 238000005406 washing Methods 0.000 description 17
- 239000007844 bleaching agent Substances 0.000 description 16
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 14
- 238000011161 development Methods 0.000 description 14
- 125000000623 heterocyclic group Chemical group 0.000 description 13
- 230000008569 process Effects 0.000 description 12
- 206010070834 Sensitisation Diseases 0.000 description 11
- 230000008313 sensitization Effects 0.000 description 11
- 230000000694 effects Effects 0.000 description 10
- 238000011160 research Methods 0.000 description 10
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 9
- 125000001931 aliphatic group Chemical group 0.000 description 9
- 125000001424 substituent group Chemical group 0.000 description 9
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Inorganic materials [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 description 8
- 239000013078 crystal Substances 0.000 description 7
- 239000000126 substance Substances 0.000 description 7
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 6
- 239000007788 liquid Substances 0.000 description 6
- DZVCFNFOPIZQKX-LTHRDKTGSA-M merocyanine Chemical compound [Na+].O=C1N(CCCC)C(=O)N(CCCC)C(=O)C1=C\C=C\C=C/1N(CCCS([O-])(=O)=O)C2=CC=CC=C2O\1 DZVCFNFOPIZQKX-LTHRDKTGSA-M 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 239000012452 mother liquor Substances 0.000 description 6
- IOLCXVTUBQKXJR-UHFFFAOYSA-M potassium bromide Chemical compound [K+].[Br-] IOLCXVTUBQKXJR-UHFFFAOYSA-M 0.000 description 6
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 6
- 230000002829 reductive effect Effects 0.000 description 6
- QGKMIGUHVLGJBR-UHFFFAOYSA-M (4z)-1-(3-methylbutyl)-4-[[1-(3-methylbutyl)quinolin-1-ium-4-yl]methylidene]quinoline;iodide Chemical compound [I-].C12=CC=CC=C2N(CCC(C)C)C=CC1=CC1=CC=[N+](CCC(C)C)C2=CC=CC=C12 QGKMIGUHVLGJBR-UHFFFAOYSA-M 0.000 description 5
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- 239000002516 radical scavenger Substances 0.000 description 5
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 4
- QIGBRXMKCJKVMJ-UHFFFAOYSA-N Hydroquinone Chemical compound OC1=CC=C(O)C=C1 QIGBRXMKCJKVMJ-UHFFFAOYSA-N 0.000 description 4
- 150000007513 acids Chemical class 0.000 description 4
- 125000002947 alkylene group Chemical group 0.000 description 4
- XYXNTHIYBIDHGM-UHFFFAOYSA-N ammonium thiosulfate Chemical compound [NH4+].[NH4+].[O-]S([O-])(=O)=S XYXNTHIYBIDHGM-UHFFFAOYSA-N 0.000 description 4
- 238000009835 boiling Methods 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- 238000005859 coupling reaction Methods 0.000 description 4
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 description 4
- 125000005843 halogen group Chemical group 0.000 description 4
- 229910052742 iron Inorganic materials 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- ADZWSOLPGZMUMY-UHFFFAOYSA-M silver bromide Chemical compound [Ag]Br ADZWSOLPGZMUMY-UHFFFAOYSA-M 0.000 description 4
- 239000011734 sodium Substances 0.000 description 4
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 description 4
- 230000000087 stabilizing effect Effects 0.000 description 4
- 239000004094 surface-active agent Substances 0.000 description 4
- 239000008399 tap water Substances 0.000 description 4
- 235000020679 tap water Nutrition 0.000 description 4
- 150000003585 thioureas Chemical class 0.000 description 4
- 239000006097 ultraviolet radiation absorber Substances 0.000 description 4
- ZRHUHDUEXWHZMA-UHFFFAOYSA-N 1,4-dihydropyrazol-5-one Chemical compound O=C1CC=NN1 ZRHUHDUEXWHZMA-UHFFFAOYSA-N 0.000 description 3
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 3
- CDAWCLOXVUBKRW-UHFFFAOYSA-N 2-aminophenol Chemical compound NC1=CC=CC=C1O CDAWCLOXVUBKRW-UHFFFAOYSA-N 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 3
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 3
- AVXURJPOCDRRFD-UHFFFAOYSA-N Hydroxylamine Chemical compound ON AVXURJPOCDRRFD-UHFFFAOYSA-N 0.000 description 3
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 3
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- RWRDLPDLKQPQOW-UHFFFAOYSA-N Pyrrolidine Chemical compound C1CCNC1 RWRDLPDLKQPQOW-UHFFFAOYSA-N 0.000 description 3
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 3
- 239000000654 additive Substances 0.000 description 3
- 125000004397 aminosulfonyl group Chemical group NS(=O)(=O)* 0.000 description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 description 3
- 230000000844 anti-bacterial effect Effects 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- IOJUPLGTWVMSFF-UHFFFAOYSA-N benzothiazole Chemical class C1=CC=C2SC=NC2=C1 IOJUPLGTWVMSFF-UHFFFAOYSA-N 0.000 description 3
- 239000011575 calcium Substances 0.000 description 3
- 125000003917 carbamoyl group Chemical group [H]N([H])C(*)=O 0.000 description 3
- 239000002738 chelating agent Substances 0.000 description 3
- 239000003638 chemical reducing agent Substances 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical class OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 238000004040 coloring Methods 0.000 description 3
- 230000008878 coupling Effects 0.000 description 3
- 238000010168 coupling process Methods 0.000 description 3
- 125000004093 cyano group Chemical group *C#N 0.000 description 3
- 125000004122 cyclic group Chemical group 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 3
- 239000000417 fungicide Substances 0.000 description 3
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 3
- 239000010413 mother solution Substances 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- 229910000027 potassium carbonate Inorganic materials 0.000 description 3
- GZTPJDLYPMPRDF-UHFFFAOYSA-N pyrrolo[3,2-c]pyrazole Chemical class N1=NC2=CC=NC2=C1 GZTPJDLYPMPRDF-UHFFFAOYSA-N 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 230000006641 stabilisation Effects 0.000 description 3
- 238000011105 stabilization Methods 0.000 description 3
- 229910052717 sulfur Inorganic materials 0.000 description 3
- 150000004764 thiosulfuric acid derivatives Chemical class 0.000 description 3
- KSDKDOFPNUJANI-UHFFFAOYSA-L trisodium sulfite Chemical compound [Na+].[Na+].[Na+].[O-]S([O-])=O KSDKDOFPNUJANI-UHFFFAOYSA-L 0.000 description 3
- KJCVRFUGPWSIIH-UHFFFAOYSA-N 1-naphthol Chemical compound C1=CC=C2C(O)=CC=CC2=C1 KJCVRFUGPWSIIH-UHFFFAOYSA-N 0.000 description 2
- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 description 2
- LMSDCGXQALIMLM-UHFFFAOYSA-N 2-[2-[bis(carboxymethyl)amino]ethyl-(carboxymethyl)amino]acetic acid;iron Chemical compound [Fe].OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O LMSDCGXQALIMLM-UHFFFAOYSA-N 0.000 description 2
- RNMCCPMYXUKHAZ-UHFFFAOYSA-N 2-[3,3-diamino-1,2,2-tris(carboxymethyl)cyclohexyl]acetic acid Chemical compound NC1(N)CCCC(CC(O)=O)(CC(O)=O)C1(CC(O)=O)CC(O)=O RNMCCPMYXUKHAZ-UHFFFAOYSA-N 0.000 description 2
- UADWUILHKRXHMM-UHFFFAOYSA-N 2-ethylhexyl benzoate Chemical compound CCCCC(CC)COC(=O)C1=CC=CC=C1 UADWUILHKRXHMM-UHFFFAOYSA-N 0.000 description 2
- 229940106004 2-ethylhexyl benzoate Drugs 0.000 description 2
- KDCGOANMDULRCW-UHFFFAOYSA-N 7H-purine Chemical compound N1=CNC2=NC=NC2=C1 KDCGOANMDULRCW-UHFFFAOYSA-N 0.000 description 2
- DLFVBJFMPXGRIB-UHFFFAOYSA-N Acetamide Chemical compound CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 229920002284 Cellulose triacetate Polymers 0.000 description 2
- 229940126062 Compound A Drugs 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 description 2
- ZHNUHDYFZUAESO-UHFFFAOYSA-N Formamide Chemical compound NC=O ZHNUHDYFZUAESO-UHFFFAOYSA-N 0.000 description 2
- YLQBMQCUIZJEEH-UHFFFAOYSA-N Furan Chemical compound C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 2
- NLDMNSXOCDLTTB-UHFFFAOYSA-N Heterophylliin A Natural products O1C2COC(=O)C3=CC(O)=C(O)C(O)=C3C3=C(O)C(O)=C(O)C=C3C(=O)OC2C(OC(=O)C=2C=C(O)C(O)=C(O)C=2)C(O)C1OC(=O)C1=CC(O)=C(O)C(O)=C1 NLDMNSXOCDLTTB-UHFFFAOYSA-N 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- SIKJAQJRHWYJAI-UHFFFAOYSA-N Indole Chemical compound C1=CC=C2NC=CC2=C1 SIKJAQJRHWYJAI-UHFFFAOYSA-N 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
- YNAVUWVOSKDBBP-UHFFFAOYSA-N Morpholine Chemical compound C1COCCN1 YNAVUWVOSKDBBP-UHFFFAOYSA-N 0.000 description 2
- CWNSVVHTTQBGQB-UHFFFAOYSA-N N,N-Diethyldodecanamide Chemical compound CCCCCCCCCCCC(=O)N(CC)CC CWNSVVHTTQBGQB-UHFFFAOYSA-N 0.000 description 2
- WTBIAPVQQBCLFP-UHFFFAOYSA-N N.N.N.CC(O)=O.CC(O)=O.CC(O)=O.CC(O)=O.CC(O)=O Chemical compound N.N.N.CC(O)=O.CC(O)=O.CC(O)=O.CC(O)=O.CC(O)=O WTBIAPVQQBCLFP-UHFFFAOYSA-N 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 2
- OFBQJSOFQDEBGM-UHFFFAOYSA-N Pentane Chemical compound CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- GLUUGHFHXGJENI-UHFFFAOYSA-N Piperazine Chemical compound C1CNCCN1 GLUUGHFHXGJENI-UHFFFAOYSA-N 0.000 description 2
- NQRYJNQNLNOLGT-UHFFFAOYSA-N Piperidine Chemical compound C1CCNCC1 NQRYJNQNLNOLGT-UHFFFAOYSA-N 0.000 description 2
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 2
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 2
- SMWDFEZZVXVKRB-UHFFFAOYSA-N Quinoline Chemical compound N1=CC=CC2=CC=CC=C21 SMWDFEZZVXVKRB-UHFFFAOYSA-N 0.000 description 2
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 description 2
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- YTPLMLYBLZKORZ-UHFFFAOYSA-N Thiophene Chemical compound C=1C=CSC=1 YTPLMLYBLZKORZ-UHFFFAOYSA-N 0.000 description 2
- UYXTWWCETRIEDR-UHFFFAOYSA-N Tributyrin Chemical compound CCCC(=O)OCC(OC(=O)CCC)COC(=O)CCC UYXTWWCETRIEDR-UHFFFAOYSA-N 0.000 description 2
- NNLVGZFZQQXQNW-ADJNRHBOSA-N [(2r,3r,4s,5r,6s)-4,5-diacetyloxy-3-[(2s,3r,4s,5r,6r)-3,4,5-triacetyloxy-6-(acetyloxymethyl)oxan-2-yl]oxy-6-[(2r,3r,4s,5r,6s)-4,5,6-triacetyloxy-2-(acetyloxymethyl)oxan-3-yl]oxyoxan-2-yl]methyl acetate Chemical compound O([C@@H]1O[C@@H]([C@H]([C@H](OC(C)=O)[C@H]1OC(C)=O)O[C@H]1[C@@H]([C@@H](OC(C)=O)[C@H](OC(C)=O)[C@@H](COC(C)=O)O1)OC(C)=O)COC(=O)C)[C@@H]1[C@@H](COC(C)=O)O[C@@H](OC(C)=O)[C@H](OC(C)=O)[C@H]1OC(C)=O NNLVGZFZQQXQNW-ADJNRHBOSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 125000003277 amino group Chemical group 0.000 description 2
- SWLVFNYSXGMGBS-UHFFFAOYSA-N ammonium bromide Chemical compound [NH4+].[Br-] SWLVFNYSXGMGBS-UHFFFAOYSA-N 0.000 description 2
- 150000003863 ammonium salts Chemical class 0.000 description 2
- 239000003242 anti bacterial agent Substances 0.000 description 2
- 230000000843 anti-fungal effect Effects 0.000 description 2
- 229940121375 antifungal agent Drugs 0.000 description 2
- 150000001556 benzimidazoles Chemical class 0.000 description 2
- UADWUILHKRXHMM-ZDUSSCGKSA-N benzoflex 181 Natural products CCCC[C@H](CC)COC(=O)C1=CC=CC=C1 UADWUILHKRXHMM-ZDUSSCGKSA-N 0.000 description 2
- 150000001558 benzoic acid derivatives Chemical class 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 150000001661 cadmium Chemical class 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- YCIMNLLNPGFGHC-UHFFFAOYSA-N catechol Chemical compound OC1=CC=CC=C1O YCIMNLLNPGFGHC-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 229910017052 cobalt Inorganic materials 0.000 description 2
- 239000010941 cobalt Substances 0.000 description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 2
- 230000002860 competitive effect Effects 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 125000000113 cyclohexyl group Chemical group [H]C1([H])C([H])([H])C([H])([H])C([H])(*)C([H])([H])C1([H])[H] 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 description 2
- 125000002228 disulfide group Chemical group 0.000 description 2
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 2
- FKRCODPIKNYEAC-UHFFFAOYSA-N ethyl propionate Chemical compound CCOC(=O)CC FKRCODPIKNYEAC-UHFFFAOYSA-N 0.000 description 2
- 230000001747 exhibiting effect Effects 0.000 description 2
- LNTHITQWFMADLM-UHFFFAOYSA-N gallic acid Chemical compound OC(=O)C1=CC(O)=C(O)C(O)=C1 LNTHITQWFMADLM-UHFFFAOYSA-N 0.000 description 2
- 229910052736 halogen Inorganic materials 0.000 description 2
- 125000005842 heteroatom Chemical group 0.000 description 2
- 150000002430 hydrocarbons Chemical group 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- RKJUIXBNRJVNHR-UHFFFAOYSA-N indolenine group Chemical group N1=CCC2=CC=CC=C12 RKJUIXBNRJVNHR-UHFFFAOYSA-N 0.000 description 2
- 239000003112 inhibitor Substances 0.000 description 2
- 150000004694 iodide salts Chemical class 0.000 description 2
- 239000004816 latex Substances 0.000 description 2
- 229920000126 latex Polymers 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- LQNUZADURLCDLV-UHFFFAOYSA-N nitrobenzene Chemical compound [O-][N+](=O)C1=CC=CC=C1 LQNUZADURLCDLV-UHFFFAOYSA-N 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- JRKICGRDRMAZLK-UHFFFAOYSA-L persulfate group Chemical group S(=O)(=O)([O-])OOS(=O)(=O)[O-] JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 description 2
- CMCWWLVWPDLCRM-UHFFFAOYSA-N phenidone Chemical compound N1C(=O)CCN1C1=CC=CC=C1 CMCWWLVWPDLCRM-UHFFFAOYSA-N 0.000 description 2
- 235000021317 phosphate Nutrition 0.000 description 2
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 2
- 239000004926 polymethyl methacrylate Substances 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 239000003755 preservative agent Substances 0.000 description 2
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 2
- WQGWDDDVZFFDIG-UHFFFAOYSA-N pyrogallol Chemical compound OC1=CC=CC(O)=C1O WQGWDDDVZFFDIG-UHFFFAOYSA-N 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 229910052711 selenium Inorganic materials 0.000 description 2
- 239000011669 selenium Substances 0.000 description 2
- NDVLTYZPCACLMA-UHFFFAOYSA-N silver oxide Chemical compound [O-2].[Ag+].[Ag+] NDVLTYZPCACLMA-UHFFFAOYSA-N 0.000 description 2
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- DLAHAXOYRFRPFQ-UHFFFAOYSA-N dodecyl benzoate Chemical compound CCCCCCCCCCCCOC(=O)C1=CC=CC=C1 DLAHAXOYRFRPFQ-UHFFFAOYSA-N 0.000 description 1
- 229940106055 dodecyl benzoate Drugs 0.000 description 1
- 125000003438 dodecyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- KWKXNDCHNDYVRT-UHFFFAOYSA-N dodecylbenzene Chemical compound CCCCCCCCCCCCC1=CC=CC=C1 KWKXNDCHNDYVRT-UHFFFAOYSA-N 0.000 description 1
- 238000000921 elemental analysis Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- DEFVIWRASFVYLL-UHFFFAOYSA-N ethylene glycol bis(2-aminoethyl)tetraacetic acid Chemical compound OC(=O)CN(CC(O)=O)CCOCCOCCN(CC(O)=O)CC(O)=O DEFVIWRASFVYLL-UHFFFAOYSA-N 0.000 description 1
- 125000006125 ethylsulfonyl group Chemical group 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- YAGKRVSRTSUGEY-UHFFFAOYSA-N ferricyanide Chemical compound [Fe+3].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-] YAGKRVSRTSUGEY-UHFFFAOYSA-N 0.000 description 1
- 238000005189 flocculation Methods 0.000 description 1
- 230000016615 flocculation Effects 0.000 description 1
- 125000002485 formyl group Chemical group [H]C(*)=O 0.000 description 1
- 235000011389 fruit/vegetable juice Nutrition 0.000 description 1
- 230000006870 function Effects 0.000 description 1
- 230000000855 fungicidal effect Effects 0.000 description 1
- 108700039708 galantide Proteins 0.000 description 1
- 229940074391 gallic acid Drugs 0.000 description 1
- 235000004515 gallic acid Nutrition 0.000 description 1
- 230000026030 halogenation Effects 0.000 description 1
- 238000005658 halogenation reaction Methods 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 description 1
- 125000004051 hexyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- WUWHPEZEVZLKEJ-UHFFFAOYSA-N hydrazine;sulfurous acid Chemical class NN.OS(O)=O WUWHPEZEVZLKEJ-UHFFFAOYSA-N 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000003840 hydrochlorides Chemical class 0.000 description 1
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 125000004029 hydroxymethyl group Chemical group [H]OC([H])([H])* 0.000 description 1
- 238000003384 imaging method Methods 0.000 description 1
- 150000002460 imidazoles Chemical class 0.000 description 1
- 230000001771 impaired effect Effects 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- QNXSIUBBGPHDDE-UHFFFAOYSA-N indan-1-one Chemical compound C1=CC=C2C(=O)CCC2=C1 QNXSIUBBGPHDDE-UHFFFAOYSA-N 0.000 description 1
- PZOUSPYUWWUPPK-UHFFFAOYSA-N indole Natural products CC1=CC=CC2=C1C=CN2 PZOUSPYUWWUPPK-UHFFFAOYSA-N 0.000 description 1
- 150000002475 indoles Chemical class 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- 239000011630 iodine Substances 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 150000002503 iridium Chemical class 0.000 description 1
- 229910052741 iridium Inorganic materials 0.000 description 1
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 description 1
- 159000000014 iron salts Chemical class 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- ZLTPDFXIESTBQG-UHFFFAOYSA-N isothiazole Chemical compound C=1C=NSC=1 ZLTPDFXIESTBQG-UHFFFAOYSA-N 0.000 description 1
- MGIYRDNGCNKGJU-UHFFFAOYSA-N isothiazolinone Chemical compound O=C1C=CSN1 MGIYRDNGCNKGJU-UHFFFAOYSA-N 0.000 description 1
- 150000002541 isothioureas Chemical class 0.000 description 1
- CTAPFRYPJLPFDF-UHFFFAOYSA-N isoxazole Chemical compound C=1C=NOC=1 CTAPFRYPJLPFDF-UHFFFAOYSA-N 0.000 description 1
- 239000003446 ligand Substances 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 125000005647 linker group Chemical group 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 229910001425 magnesium ion Inorganic materials 0.000 description 1
- 239000001630 malic acid Chemical class 0.000 description 1
- 235000011090 malic acid Nutrition 0.000 description 1
- 150000002736 metal compounds Chemical class 0.000 description 1
- 125000001434 methanylylidene group Chemical group [H]C#[*] 0.000 description 1
- 125000000956 methoxy group Chemical group [H]C([H])([H])O* 0.000 description 1
- 125000004170 methylsulfonyl group Chemical group [H]C([H])([H])S(*)(=O)=O 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 125000006518 morpholino carbonyl group Chemical group [H]C1([H])OC([H])([H])C([H])([H])N(C(*)=O)C1([H])[H] 0.000 description 1
- NPKFETRYYSUTEC-UHFFFAOYSA-N n-[2-(4-amino-n-ethyl-3-methylanilino)ethyl]methanesulfonamide Chemical compound CS(=O)(=O)NCCN(CC)C1=CC=C(N)C(C)=C1 NPKFETRYYSUTEC-UHFFFAOYSA-N 0.000 description 1
- SXHIEJQAGMGCQR-UHFFFAOYSA-N n-methylaniline;sulfuric acid Chemical compound OS(O)(=O)=O.CNC1=CC=CC=C1 SXHIEJQAGMGCQR-UHFFFAOYSA-N 0.000 description 1
- PCILLCXFKWDRMK-UHFFFAOYSA-N naphthalene-1,4-diol Chemical compound C1=CC=C2C(O)=CC=C(O)C2=C1 PCILLCXFKWDRMK-UHFFFAOYSA-N 0.000 description 1
- 125000001624 naphthyl group Chemical group 0.000 description 1
- 125000004957 naphthylene group Chemical group 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- MGFYIUFZLHCRTH-UHFFFAOYSA-N nitrilotriacetic acid Chemical compound OC(=O)CN(CC(O)=O)CC(O)=O MGFYIUFZLHCRTH-UHFFFAOYSA-N 0.000 description 1
- 150000002828 nitro derivatives Chemical class 0.000 description 1
- 125000000449 nitro group Chemical group [O-][N+](*)=O 0.000 description 1
- 125000004433 nitrogen atom Chemical group N* 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 239000002667 nucleating agent Substances 0.000 description 1
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 1
- 125000002347 octyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 150000002916 oxazoles Chemical class 0.000 description 1
- 150000002918 oxazolines Chemical class 0.000 description 1
- AHHWIHXENZJRFG-UHFFFAOYSA-N oxetane Chemical compound C1COC1 AHHWIHXENZJRFG-UHFFFAOYSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- 150000004989 p-phenylenediamines Chemical class 0.000 description 1
- 235000019629 palatability Nutrition 0.000 description 1
- 125000000913 palmityl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 239000012188 paraffin wax Substances 0.000 description 1
- 229960003330 pentetic acid Drugs 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 150000004965 peroxy acids Chemical class 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- WVDDGKGOMKODPV-ZQBYOMGUSA-N phenyl(114C)methanol Chemical compound O[14CH2]C1=CC=CC=C1 WVDDGKGOMKODPV-ZQBYOMGUSA-N 0.000 description 1
- 125000000843 phenylene group Chemical group C1(=C(C=CC=C1)*)* 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- ZJAOAACCNHFJAH-UHFFFAOYSA-N phosphonoformic acid Chemical class OC(=O)P(O)(O)=O ZJAOAACCNHFJAH-UHFFFAOYSA-N 0.000 description 1
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 1
- 150000003021 phthalic acid derivatives Chemical class 0.000 description 1
- XKJCHHZQLQNZHY-UHFFFAOYSA-N phthalimide Chemical compound C1=CC=C2C(=O)NC(=O)C2=C1 XKJCHHZQLQNZHY-UHFFFAOYSA-N 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 229920000172 poly(styrenesulfonic acid) Polymers 0.000 description 1
- 229920000768 polyamine Polymers 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 239000004848 polyfunctional curative Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 229940005642 polystyrene sulfonic acid Drugs 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000002335 preservative effect Effects 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- NDGRWYRVNANFNB-UHFFFAOYSA-N pyrazolidin-3-one Chemical class O=C1CCNN1 NDGRWYRVNANFNB-UHFFFAOYSA-N 0.000 description 1
- USPWKWBDZOARPV-UHFFFAOYSA-N pyrazolidine Chemical compound C1CNNC1 USPWKWBDZOARPV-UHFFFAOYSA-N 0.000 description 1
- DNXIASIHZYFFRO-UHFFFAOYSA-N pyrazoline Chemical compound C1CN=NC1 DNXIASIHZYFFRO-UHFFFAOYSA-N 0.000 description 1
- MCSKRVKAXABJLX-UHFFFAOYSA-N pyrazolo[3,4-d]triazole Chemical compound N1=NN=C2N=NC=C21 MCSKRVKAXABJLX-UHFFFAOYSA-N 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 150000003222 pyridines Chemical class 0.000 description 1
- 229940079877 pyrogallol Drugs 0.000 description 1
- ZVJHJDDKYZXRJI-UHFFFAOYSA-N pyrroline Natural products C1CC=NC1 ZVJHJDDKYZXRJI-UHFFFAOYSA-N 0.000 description 1
- 150000003236 pyrrolines Chemical class 0.000 description 1
- 150000003242 quaternary ammonium salts Chemical class 0.000 description 1
- 150000003248 quinolines Chemical class 0.000 description 1
- 150000004053 quinones Chemical class 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- KIWUVOGUEXMXSV-UHFFFAOYSA-N rhodanine Chemical class O=C1CSC(=S)N1 KIWUVOGUEXMXSV-UHFFFAOYSA-N 0.000 description 1
- 150000003283 rhodium Chemical class 0.000 description 1
- 230000005070 ripening Effects 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 229940116351 sebacate Drugs 0.000 description 1
- CXMXRPHRNRROMY-UHFFFAOYSA-L sebacate(2-) Chemical compound [O-]C(=O)CCCCCCCCC([O-])=O CXMXRPHRNRROMY-UHFFFAOYSA-L 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 1
- 229910001923 silver oxide Inorganic materials 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- QHFDHWJHIAVELW-UHFFFAOYSA-M sodium;4,6-dioxo-1h-1,3,5-triazin-2-olate Chemical class [Na+].[O-]C1=NC(=O)NC(=O)N1 QHFDHWJHIAVELW-UHFFFAOYSA-M 0.000 description 1
- 239000012798 spherical particle Substances 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 125000004079 stearyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 125000005504 styryl group Chemical group 0.000 description 1
- 229960002317 succinimide Drugs 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-L sulfite Chemical class [O-]S([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-L 0.000 description 1
- HXJUTPCZVOIRIF-UHFFFAOYSA-N sulfolane Chemical compound O=S1(=O)CCCC1 HXJUTPCZVOIRIF-UHFFFAOYSA-N 0.000 description 1
- 125000000472 sulfonyl group Chemical group *S(*)(=O)=O 0.000 description 1
- XIUROWKZWPIAIB-UHFFFAOYSA-N sulfotep Chemical compound CCOP(=S)(OCC)OP(=S)(OCC)OCC XIUROWKZWPIAIB-UHFFFAOYSA-N 0.000 description 1
- 125000004434 sulfur atom Chemical group 0.000 description 1
- 239000011975 tartaric acid Chemical class 0.000 description 1
- 235000002906 tartaric acid Nutrition 0.000 description 1
- RAOIDOHSFRTOEL-UHFFFAOYSA-N tetrahydrothiophene Chemical compound C1CCSC1 RAOIDOHSFRTOEL-UHFFFAOYSA-N 0.000 description 1
- 150000003475 thallium Chemical class 0.000 description 1
- 150000003557 thiazoles Chemical class 0.000 description 1
- 150000003549 thiazolines Chemical class 0.000 description 1
- VOVUARRWDCVURC-UHFFFAOYSA-N thiirane Chemical compound C1CS1 VOVUARRWDCVURC-UHFFFAOYSA-N 0.000 description 1
- 150000003556 thioamides Chemical class 0.000 description 1
- 150000003567 thiocyanates Chemical class 0.000 description 1
- 150000003568 thioethers Chemical class 0.000 description 1
- 229930192474 thiophene Natural products 0.000 description 1
- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical class CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 description 1
- IELLVVGAXDLVSW-UHFFFAOYSA-N tricyclohexyl phosphate Chemical compound C1CCCCC1OP(OC1CCCCC1)(=O)OC1CCCCC1 IELLVVGAXDLVSW-UHFFFAOYSA-N 0.000 description 1
- OHRVKCZTBPSUIK-UHFFFAOYSA-N tridodecyl phosphate Chemical compound CCCCCCCCCCCCOP(=O)(OCCCCCCCCCCCC)OCCCCCCCCCCCC OHRVKCZTBPSUIK-UHFFFAOYSA-N 0.000 description 1
- APVVRLGIFCYZHJ-UHFFFAOYSA-N trioctyl 2-hydroxypropane-1,2,3-tricarboxylate Chemical compound CCCCCCCCOC(=O)CC(O)(C(=O)OCCCCCCCC)CC(=O)OCCCCCCCC APVVRLGIFCYZHJ-UHFFFAOYSA-N 0.000 description 1
- WTLBZVNBAKMVDP-UHFFFAOYSA-N tris(2-butoxyethyl) phosphate Chemical compound CCCCOCCOP(=O)(OCCOCCCC)OCCOCCCC WTLBZVNBAKMVDP-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 150000003673 urethanes Chemical class 0.000 description 1
- 150000003751 zinc Chemical class 0.000 description 1
Classifications
-
- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03C—PHOTOSENSITIVE MATERIALS FOR PHOTOGRAPHIC PURPOSES; PHOTOGRAPHIC PROCESSES, e.g. CINE, X-RAY, COLOUR, STEREO-PHOTOGRAPHIC PROCESSES; AUXILIARY PROCESSES IN PHOTOGRAPHY
- G03C7/00—Multicolour photographic processes or agents therefor; Regeneration of such processing agents; Photosensitive materials for multicolour processes
- G03C7/30—Colour processes using colour-coupling substances; Materials therefor; Preparing or processing such materials
- G03C7/3029—Materials characterised by a specific arrangement of layers, e.g. unit layers, or layers having a specific function
Landscapes
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Silver Salt Photography Or Processing Solution Therefor (AREA)
Abstract
Description
【発明の詳細な説明】
(産業上の利用分野)
本発明は、高感度のカラーネガ感光材料に関し特に脱銀
が容易で迅速処理に適したカラーネガ感光材料に関する
。DETAILED DESCRIPTION OF THE INVENTION (Field of Industrial Application) The present invention relates to a highly sensitive color negative light-sensitive material, and particularly to a color negative light-sensitive material that is easy to desilver and suitable for rapid processing.
(従来の技術)
近年、撮影用感光材料の技術の進歩により、高感度の感
光材料が次々と発売されている。暗い室内などでのスト
ロボを使わない撮影、スポーツ写真などでの望遠レンズ
を用いた高速シャッターでの撮影、天文写真など長時間
露光を必要とする撮影など感光材料の高感度化による撮
影領域の拡大は、当業界に課せられた永遠のテーマであ
る。(Prior Art) In recent years, with advances in the technology of photographic photosensitive materials, highly sensitive photosensitive materials have been released one after another. Expanding the range of photography by increasing the sensitivity of photosensitive materials, such as shooting without a strobe in a dark room, shooting with a high-speed shutter using a telephoto lens for sports photography, and shooting that requires long exposures such as astronomical photography. is an eternal theme for this industry.
感光材料の高感度化のために、これまで多くの努力がな
されてきた。ハロゲン化銀粒子の形状、組成などの形成
方法、化学増感、分光増感、添加剤、カプラー構造など
について数多くの研究が行なわれ、有益な発明がいくつ
かなされている。しかしながら、高感度感光材料に関す
る要求は技術の進歩以上に大きく、これらの方法だけで
は残念ながら充分とは言えなかった。そこで高感度化の
ためにハロゲン化銀乳剤粒子のサイズを大きくする、と
いう方法を他の技術と併用して高感度感光材料を作るの
が当業界での常套手段となっている。Many efforts have been made to increase the sensitivity of photosensitive materials. Numerous studies have been conducted on formation methods such as the shape and composition of silver halide grains, chemical sensitization, spectral sensitization, additives, coupler structures, etc., and several useful inventions have been made. However, the demands for highly sensitive photosensitive materials are greater than the advances in technology, and unfortunately these methods alone have not been sufficient. Therefore, it has become common practice in the industry to increase the size of silver halide emulsion grains in combination with other techniques to produce high-sensitivity light-sensitive materials in order to increase sensitivity.
ハロゲン化銀乳剤粒子のサイズを大きくするとある程度
までは感度が上昇するが、ハロゲン化銀の含有量を一定
に保っている限り、必然的にハロゲン化銀乳剤粒子数の
減少、したがって現像開始点の数が減少し、粒状性が大
きく損われるという大きな欠点がある。この欠点を補う
ために、英国特許筒923.045号、特公昭49−1
5495号公報に記載されているような、同一感色性を
持ち感度、すなわちハロゲン化銀の粒子サイズが異なる
二つ以上の乳剤層を有する感光材料、特開昭55−62
454号公報等に記載されているような高速反応性カプ
ラーを用いる方法、米国特許第3.227,554号、
米国特許第3,632゜435号等に記載されているよ
うないわゆるDIRカプラー、DIR化合物を用いる方
法、英国特許筒2,083,640号に記載の移動性の
色素を生じるようなカプラーを用いる方法、特開昭60
−128443号公報に記載の平均沃化銀含有率の高い
ハロゲン化銀を用いる方法などが知られている。これら
の方法はそれぞれ大きな効果があるすぐれた発明である
が、高感度でかつ高画質を求める大きな要求に対しては
、充分な技術ではなかった。そこで、ハロゲン化銀乳剤
粒子の粒子サイズを大きくすると同時に、現像開始点の
数を少しでも増加させるために、高感度のカラーネガ感
光材料は漂白定着処理時の脱銀性などの諸性能が許され
る範囲でハロゲン化銀乳剤粒子の含有量を多くした設計
がなされてきた。Increasing the size of the silver halide emulsion grains increases the sensitivity to a certain extent, but as long as the silver halide content is kept constant, the number of silver halide emulsion grains inevitably decreases, and therefore the development starting point increases. The major disadvantage is that the number is reduced and the graininess is greatly impaired. In order to compensate for this drawback, British Patent No. 923.045,
A photographic material having two or more emulsion layers having the same color sensitivity and different sensitivities, that is, different silver halide grain sizes, as described in JP-A No. 5495, JP-A-55-62
Methods using fast-reactive couplers such as those described in US Pat. No. 454, US Pat. No. 3,227,554,
Methods using so-called DIR couplers and DIR compounds as described in U.S. Pat. Method, Japanese Unexamined Patent Publication 1986
A method using silver halide having a high average silver iodide content is known, as described in Japanese Patent No. 128443. Although each of these methods is an excellent invention with great effects, they are not sufficient technologies to meet the great demand for high sensitivity and high image quality. Therefore, in order to increase the grain size of silver halide emulsion grains and at the same time increase the number of development initiation points even slightly, high-sensitivity color negative light-sensitive materials are required to have various performances such as desilvering properties during bleach-fixing processing. Designs have been made in which the content of silver halide emulsion grains is increased within a range.
一方、高感度のカラーネガ感光材料において高感度の実
現のため、あるいは高感度と高画質の両立のために多層
よりなるカラーネガ感光材料の層の位置を変更すること
が知られていた。例えば米国特許第4,184.876
号、第4.129゜446号、第4,186,016号
、英国特許筒1.560,965号、米国特許第4,1
86゜011号、第4,267.264号、第4,17
3.479号、第4,157,917号、第4゜165
.236号、英国特許筒2. 138. 962号、特
開昭59−177.552号、英国特許筒2.137.
372号、特開昭59−180゜555号、特開昭59
−180,556号、59−204,038号などに記
述されている。On the other hand, it has been known to change the positions of the layers of a multilayer color negative photosensitive material in order to achieve high sensitivity or to achieve both high sensitivity and high image quality. For example, U.S. Patent No. 4,184.876
No. 4.129°446, No. 4,186,016, British Patent No. 1.560,965, U.S. Patent No. 4.1
86゜011, No. 4,267.264, No. 4,17
No. 3.479, No. 4,157,917, No. 4゜165
.. No. 236, British patent cylinder 2. 138. No. 962, JP-A-59-177.552, British Patent No. 2.137.
No. 372, JP-A-59-180゜555, JP-A-59
It is described in No. 180,556, No. 59-204,038, etc.
これらの技術は前記特開昭59−177.552号など
に記述されているように支持体により近い側にある乳剤
層はより遠い側にある乳剤層の影響により露光量のロス
および現像の遅れがおこり低感、軟調になってしまうこ
とが知られているので通常より支持体に近い側に位置す
る赤感性乳剤層および/または緑感性乳剤層の各々の最
も高感度の乳剤層をなるべく支持体より遠くに位置させ
ることにより、高感度化を達成しようとするものである
。As described in JP-A-59-177.552, the emulsion layer closer to the support is affected by the emulsion layer farther away, resulting in a loss in exposure and a delay in development. It is known that this can result in low sensitivity and soft tone, so it is best to support the most sensitive emulsion layer of each of the red-sensitive emulsion layer and/or green-sensitive emulsion layer, which are located closer to the support than usual. The aim is to achieve high sensitivity by locating it far from the body.
一方、上記のような高感度の盪影材料は報道分野で多く
使用され、特に処理の迅速化が求められている。On the other hand, high-sensitivity imaging materials such as those described above are often used in the news field, and there is a particular need for speedy processing.
従来の処理工程では脱銀や定着工程の占める割り合いが
高く迅速化のためには漂白や定着工程を短縮する必要が
あった。このような工程時間の短縮は、大サイズのハロ
ゲン化銀を利用し、高銀量で厚膜の高感度カラー感光材
料には特に不利で脱銀不良をまねきやすい。In conventional processing processes, the desilvering and fixing steps account for a large proportion of the time, and in order to speed up processing, it was necessary to shorten the bleaching and fixing steps. Such reduction in process time is particularly disadvantageous for high-sensitivity color photosensitive materials that utilize large-sized silver halide, have a high silver content, and are thick, and are likely to cause desilvering defects.
(発明が解決しようとする問題点)
先に述べた高感度の乳剤層を支持体より遠くに位置させ
る構成のカラー感光材料は、感色性の異なる乳剤層を隔
てる中間層の数が増加し、層間混色を防止するため、現
像主薬酸化体のスカベンジャーを多用するので更に高銀
、厚膜となりやすく、処理の迅速化には著るしく不利で
あった。(Problems to be Solved by the Invention) In the color light-sensitive materials described above in which the highly sensitive emulsion layer is located far from the support, the number of intermediate layers separating the emulsion layers with different color sensitivities increases. In order to prevent interlayer color mixing, a scavenger for the oxidized developing agent is frequently used, which tends to result in a higher silver content and thicker film, which is extremely disadvantageous for speeding up processing.
そこで感光材料の中に漂白剤や、漂白促進剤もしくはそ
れらのプレカーサーを内蔵させ脱銀を促進させようとす
る試がなされてきた。リサーチ・ディスクロージャーI
tem Na24241号、同11449号及び特開
昭61−201247号明細書に漂白促進化合物放出型
カプラーに関する記載があり、かかる漂白促進化合物放
出型カプラーを含有するハロゲン化銀カラー写真感光材
料を用いることによりその脱銀性が改良されることが知
られている。Therefore, attempts have been made to incorporate bleaching agents, bleach accelerators, or their precursors into photosensitive materials to accelerate desilvering. Research Disclosure I
tem Na24241, No. 11449, and JP-A-61-201247 disclose bleach-accelerating compound-releasing couplers, and by using silver halide color photographic light-sensitive materials containing such bleach-accelerating compound-releasing couplers, It is known that its desilvering properties are improved.
しかしながら、これらのカプラーはillが4〜6 g
/rdの通常の感光材料ではその効果が充分には発揮さ
れないのに対し、先述の構成のカラー感光材料では著る
しい効果を示すことがわかった。However, these couplers have an ill of 4-6 g
It has been found that the effect is not fully exhibited in the ordinary light-sensitive material of /rd, whereas the color light-sensitive material having the above-mentioned structure exhibits a remarkable effect.
従って本発明の目的は、高感度で脱銀の容易なカラー感
光材料を提供することであり、特に高感度で迅速処理適
性のあるカラー感光材料を提供することにある。Therefore, an object of the present invention is to provide a color light-sensitive material with high sensitivity and easy desilvering, and particularly to provide a color light-sensitive material with high sensitivity and suitability for rapid processing.
(問題点を解決するための手段)
本発明の目的は、青感層、緑感層、および赤感性の各ハ
ロゲン化銀乳剤層を存し、これらのうち少くとも1つが
互いに感度の異なる2つ以上の層からなり、この2層以
上の層は支持体側からみて低感層から高感層へと順に配
列され、該低感層と高感層の間に感色性の異なるハロゲ
ン化銀乳剤層が少くとも1つ配されているカラー感光材
料が、芳香族第1級アミン現像主薬の酸化体と反応して
漂白促進剤を放出する化合物を少くとも一種含存するこ
とを特徴とするハロゲン化銀カラー感光材料によって達
成される。(Means for Solving the Problems) An object of the present invention is to provide a blue-sensitive layer, a green-sensitive layer, and a red-sensitive silver halide emulsion layer, in which at least one of these layers has two different sensitivities. The two or more layers are arranged in order from the low-sensitivity layer to the high-sensitivity layer when viewed from the support side, and between the low-sensitivity layer and the high-sensitivity layer are silver halide compounds having different color sensitivities. A halogen-based color light-sensitive material having at least one emulsion layer containing at least one compound that reacts with an oxidized product of an aromatic primary amine developing agent to release a bleaching accelerator. This can be achieved using silver oxide color photosensitive materials.
以下本発明の詳細な説明する。The present invention will be explained in detail below.
本発明の感光材料は、高画質、高感度の盪影用カラー感
光材料であり、特定写真感度が320以上であり、感光
材料中に含有されるすべての銀量が5.0〜13.0g
/nfが好ましい、特定写真感度320以下では本発明
のような層の構成をとる必要がない、また銀量が13g
/n?以上では、本発明の化合物を用いても脱銀工程の
短縮は困難である。The light-sensitive material of the present invention is a high-quality, high-sensitivity color light-sensitive material for shadowing, has a specific photographic sensitivity of 320 or higher, and has a total silver content of 5.0 to 13.0 g.
/nf is preferable, when the specific photographic sensitivity is 320 or less, it is not necessary to have a layer structure as in the present invention, and the amount of silver is 13 g.
/n? In the above, it is difficult to shorten the desilvering step even if the compound of the present invention is used.
特定写真感度の定義および測定方法については、特願昭
61−245575号7ページから17ページに記載さ
れている。The definition and measuring method of specific photographic sensitivity are described on pages 7 to 17 of Japanese Patent Application No. 61-245575.
感光材料の銀の含有量を分析するにはいくつかの方法が
公知となっており、どの方法を用いても良い。例えば蛍
光X線を用いた元素分析などが簡便である。Several methods are known for analyzing the silver content of photosensitive materials, and any method may be used. For example, elemental analysis using fluorescent X-rays is convenient.
本発明のカラーネガ感光材料の特定写真感度は、320
以上でなくてはいけない。より低感度の場合には本発明
の多層カラーネガ感光材料の層の配列順序に対する工夫
と含有される銀の量との組み合わせの効果があまり発揮
されないのである。好ましくは400以上、より好まし
くは800以上である。The specific photographic sensitivity of the color negative light-sensitive material of the present invention is 320
It has to be more than that. In the case of lower sensitivity, the effect of the combination of the arrangement order of the layers of the multilayer color negative light-sensitive material of the present invention and the amount of silver contained is not so pronounced. Preferably it is 400 or more, more preferably 800 or more.
本発明のカラーネガ感光材料は赤感性乳剤層、緑感性乳
剤層、青感性乳剤層が各々感度の異なる2層以上の乳剤
層から構成され、最も感度の高い赤感性乳剤層、最も感
度の高い緑感性乳剤層、最も感度の高い青感性乳剤層の
うち最も支持体に近い層と支持体との間に上記支持体に
最も近い最高感度層とは感色性の異なる少なくとも1つ
の乳剤層が位置する必要がある。The color negative light-sensitive material of the present invention is composed of two or more emulsion layers, each having a red-sensitive emulsion layer, a green-sensitive emulsion layer, and a blue-sensitive emulsion layer, each having a different sensitivity. At least one emulsion layer having a different color sensitivity from the highest sensitivity layer closest to the support is located between the sensitive emulsion layer, the layer closest to the support among the most sensitive blue-sensitive emulsion layers, and the support. There is a need to.
また、さらに粒状性を改良するために各々の感色性の層
を3層構成とするとさらに好ましい。この技術は、特公
昭49−15,495号に記載されている。Further, in order to further improve the graininess, it is more preferable that each color-sensitive layer has a three-layer structure. This technique is described in Japanese Patent Publication No. 49-15,495.
各感光性乳剤層の間に非感光性層が存在しても良い。こ
の非感光性層は、同じ感色性を持つ2つ以上の乳剤層の
間に存在しても良い、又、感色性の異なる感光性乳剤層
が隣接する場合にはその間に非感光性層を設けることが
好ましい、このようような非感光性中間層にスカベンジ
ャー物質を含有することもできる。また特開昭59−1
60゜135号に記述されているように感光性乳剤層の
下に非感光性反射層を設けて感度を向上させることも好
ましい、また、本発明のカラーネガ感光材料には、必ず
しも必要ではないが、通常はイエロー・フィルター層を
含有する。A non-light sensitive layer may be present between each light sensitive emulsion layer. This non-light-sensitive layer may exist between two or more emulsion layers having the same color sensitivity, or if there are adjacent light-sensitive emulsion layers with different color sensitivities, there may be a non-light-sensitive layer between them. Scavenger substances can also be included in such non-photosensitive intermediate layers, which are preferably provided. Also, JP-A-59-1
As described in No. 60°135, it is also preferable to provide a non-light-sensitive reflective layer under the light-sensitive emulsion layer to improve sensitivity. , usually containing a yellow filter layer.
本発明のカラーネガ感光材料における感光性乳剤層の層
の配列順序の具体例を以下に挙げるがこれらに限定され
るものではない。なお、非感光性層はここでは省略しで
あるが、前述した様な位置に存在させても良い。Specific examples of the arrangement order of the light-sensitive emulsion layers in the color negative light-sensitive material of the present invention are listed below, but the order is not limited thereto. Although the non-photosensitive layer is omitted here, it may be present at the position described above.
(11支持体、低感度赤感性乳剤層(以下RL)、低感
度緑感性乳剤層(以下GL)、低感度青感性乳剤層(以
下BL)、高感度赤感性乳剤層(Rf()、高感度緑感
性乳剤層(GH)、高感度青感性乳剤層(BH)。(11 supports, low sensitivity red sensitive emulsion layer (hereinafter referred to as RL), low sensitivity green sensitive emulsion layer (hereinafter referred to as GL), low sensitivity blue sensitive emulsion layer (hereinafter referred to as BL), high sensitivity red sensitive emulsion layer (Rf(), high High-speed green-sensitive emulsion layer (GH), high-speed blue-sensitive emulsion layer (BH).
(2)支持体、RLlGL、BL、GH,RH,BH(
3)支持体、RL%GL、BL、RH,中開度緑感性乳
剤層(以下GM) 、G)(、BH(4)支持体、RL
、GLSGM、BL、RH。(2) Support, RLlGL, BL, GH, RH, BH (
3) Support, RL% GL, BL, RH, medium-opening green-sensitive emulsion layer (GM), G) (, BH (4) Support, RL
, GLSGM, BL, RH.
GH,BH
(5)支持体、RL、中開度赤感性乳剤層(以下RM)
、GL、GM、BL、中開度青感性乳剤層(以下BM
) 、RHSGH,BH
(6)支持体、RL、GL、BL、RM、RH。GH, BH (5) Support, RL, medium-opening red-sensitive emulsion layer (hereinafter referred to as RM)
, GL, GM, BL, medium-opening blue-sensitive emulsion layer (hereinafter referred to as BM
), RHSGH, BH (6) Support, RL, GL, BL, RM, RH.
GM、OH,、BM、BH
(7)支持体、RL、GL、RH,GH,BL、BH(
8)支持体、GL、、RL、RH,GH,BL、BH(
9)支持体、RL、GLSRH,、GM、GH。GM, OH,, BM, BH (7) Support, RL, GL, RH, GH, BL, BH (
8) Support, GL, RL, RH, GH, BL, BH (
9) Support, RL, GLSRH, GM, GH.
BL、、BH
αψ支持体、RL%GL、、GH5RHSBL、BH本
発明のハロゲン化銀写真感光材料の写真乳剤層にはハロ
ゲン化銀として臭化銀、沃臭化銀、沃塩臭化銀、塩臭化
銀及び塩化銀のいずれを用いてもよい。好ましいハロゲ
ン化銀は30モル%以下の沃化銀を含む沃臭化銀である
。特に好ましいのは2モル%から20モル%までの沃化
銀を含む沃臭化銀である。また、高感度でかつ高画質を
両立させるためには特開昭60−128,443号公報
に記載されているように全乳剤層のハロゲン化銀の平均
沃化銀含有率を8モル%以上にするのが好ましい。ハロ
ゲン化銀の平均沃化銀含有率を上げると粒状性が顕著に
改良されることが知られているがある程度以上の沃化銀
含有率になると、現像速度の遅れ、脱銀、定着速度の遅
れなどの欠点が出てくる。BL,, BH αψ support, RL% GL,, GH5RHSBL, BH The photographic emulsion layer of the silver halide photographic light-sensitive material of the present invention contains silver bromide, silver iodobromide, silver iodochlorobromide, silver halide, Either silver chlorobromide or silver chloride may be used. A preferred silver halide is silver iodobromide containing up to 30 mole percent silver iodide. Particularly preferred is silver iodobromide containing from 2 mol % to 20 mol % silver iodide. In addition, in order to achieve both high sensitivity and high image quality, the average silver iodide content of silver halide in all emulsion layers must be 8 mol% or more, as described in JP-A-60-128,443. It is preferable to It is known that graininess is significantly improved by increasing the average silver iodide content of silver halide, but if the silver iodide content exceeds a certain level, development speed may be delayed, desilvering, and fixing speed may be reduced. There are drawbacks such as delays.
本発明のハロゲン化銀写真感光材料の写真乳剤層に用い
るハロゲン化銀粒子は、沃化銀を5モル%以上含有する
沃臭化銀から実質的に成るコアと、該コアを被覆し、沃
化銀含有率がコアの沃化銀含有率よりも低い沃臭化銀ま
たは臭化銀から実質的に成るシェルによって構成される
二重構造を有することが好ましい。コアの沃化銀含有率
は10モル%以上であることが更に好ましく、20モル
%以上44モル%以下であることがもつとも好ましい、
シェルの沃化銀含有率は5モル%以下であることが好ま
しい。The silver halide grains used in the photographic emulsion layer of the silver halide photographic light-sensitive material of the present invention include a core consisting essentially of silver iodobromide containing 5 mol% or more of silver iodide, and a core consisting essentially of silver iodobromide containing 5 mol% or more of silver iodide; It is preferred to have a double structure constituted by a shell consisting essentially of silver iodobromide or silver bromide, the silver iodide content of which is lower than the silver iodide content of the core. The silver iodide content of the core is more preferably 10 mol% or more, and even more preferably 20 mol% or more and 44 mol% or less.
The silver iodide content of the shell is preferably 5 mol% or less.
該コアは、沃化銀を均一に含んでいても良いし、又、沃
化銀含有率の異なる相から成る多重構造をもっていても
良い。後者の場合には、沃化銀含有率の最も高い相の沃
化銀含有率が5モル%以上であり、更に好ましくは10
モル%以上であり、且つ、シェルの沃化銀含有率がコア
の最高沃化銀含有率相のそれよりも低ければ良い。又、
「沃臭化銀から実質的に成る」とは、主に沃臭化銀から
成っているが、それ以外の成分も1モル%位までは含有
しても良いことを意味する。The core may contain silver iodide uniformly, or may have a multilayer structure consisting of phases having different silver iodide contents. In the latter case, the silver iodide content of the phase with the highest silver iodide content is 5 mol% or more, more preferably 10
% by mole or more, and the silver iodide content of the shell is lower than that of the highest silver iodide content phase of the core. or,
"Substantially consisting of silver iodobromide" means that it mainly consists of silver iodobromide, but may also contain up to about 1 mol % of other components.
本発明のハロゲン化銀写真感光材料の写真乳剤層に用い
るハロゲン化銀粒子のさらに好ましい態様としては、回
折角度(2θ)が38〜42°の範囲でCuのにβ線を
用いてハロゲン化銀の(220)面の回折強度対回折角
度のカーブを得た時、コア部分に相当する回折ピークと
、シェル部に相当するピークの2本の回折極大と、その
間に1つの極小があられれ、かつコア部分に相当する回
折強度が、シェル部のそれの1/10〜3/1になるよ
うな構造を有する粒子である。特に好ましくは回折強度
比が115〜3/1、さらに1/3〜3/1の場合であ
る。In a further preferred embodiment of the silver halide grains used in the photographic emulsion layer of the silver halide photographic light-sensitive material of the present invention, the silver halide grains have a diffraction angle (2θ) in the range of 38 to 42°, and the silver halide grains are When we obtain the diffraction intensity vs. diffraction angle curve for the (220) plane, we find that there are two diffraction maxima, a diffraction peak corresponding to the core part and a peak corresponding to the shell part, and one minimum between them. In addition, the particles have a structure such that the diffraction intensity corresponding to the core portion is 1/10 to 3/1 of that of the shell portion. Particularly preferably, the diffraction intensity ratio is 115 to 3/1, more preferably 1/3 to 3/1.
このような二重構造化により、現像速度の遅れをまねく
ことなく高ヨードの沃臭化銀乳剤を用いることが可能に
なり、少ない塗布銀量でもすぐれた粒状性を有する感光
材料を達成することができしかしながら、このような法
度含率の上昇は、脱銀速度の増大をもたらし、脱銀促進
技術との組み合わせが必須となる。Such a double structure makes it possible to use a high-iodine silver iodobromide emulsion without causing a delay in development speed, and it is possible to achieve a photosensitive material with excellent graininess even with a small amount of coated silver. However, such an increase in the content leads to an increase in the desilvering rate, and a combination with desilvering acceleration technology is essential.
写真乳剤中のハロゲン化!!粒子の平均粒子サイズ(球
状または球に近似の粒子の場合は粒子直径。Halogenation in photographic emulsions! ! Average particle size of particles (particle diameter for spherical or approximating spherical particles).
立方体粒子の場合は稜長を粒子サイズとし、投影面積に
もとずく平均で表わす、)は特に問わないが、0.05
μm以上10μm以下が好ましい、各々の最高感度を持
つ乳剤層中のハロゲン化銀粒子の平均サイズは、0.5
μm以上4μm以下が好ましく、0.6μm以上、2.
5μm以下がさらに好ましい。In the case of cubic particles, the particle size is defined as the edge length, and is expressed as an average based on the projected area.) is not particularly limited, but is 0.05
The average size of silver halide grains in each emulsion layer having the highest sensitivity is preferably 0.5 μm or more and 10 μm or less.
The range is preferably 0.6 μm or more, 2.
More preferably, the thickness is 5 μm or less.
粒子サイズは狭くても広くてもいずれでもよい。The particle size may be narrow or wide.
写真乳剤中のハロゲン化銀粒子は、立方体、へ方体のよ
゛うな規則的な結晶体を有するものでもよく、また球状
、板状などのような変則的な結1品体を持つもの、或い
はこれらの結晶形の複合形・でもよい0種々の結晶形の
粒子の混合から成ってもより1゜
また増感色素による色増感効率の高い、アスペクト比が
5以上であるような平板状粒子を使うのは好ましい。The silver halide grains in the photographic emulsion may have a regular crystal structure such as a cube or a rectangular shape, or may have an irregular crystal structure such as a spherical shape or a plate shape. Alternatively, it may be a composite form of these crystal forms.Also, it may be a mixture of particles of various crystal forms, but it may be a flat plate with an aspect ratio of 5 or more, which has a high color sensitization efficiency with a sensitizing dye. Preferably, particles are used.
平板状粒子は、ガトフ著、フオトグラフイク・サイエン
ス・アンド・エンジニアリング(Gutoff+Pho
to(Hraphic 5cience and En
(Hineering) 、第14巻、248〜257
頁(1970年):米国特許第4,434,226号、
同4,414,310号、同4,433.048号、同
4,439,520号および英国特許第2,112,1
57号などに記載の方法により簡囃に調製することがで
きる。Tabular grains are described in Gutoff, Photographic Science and Engineering (Gutoff+Pho).
to(Hraphic 5science and En
(Hineering), Volume 14, 248-257
Page (1970): U.S. Patent No. 4,434,226;
4,414,310, 4,433.048, 4,439,520 and British Patent No. 2,112,1
It can be easily prepared by the method described in No. 57, etc.
本発明に用いられる写真乳剤はP、 Glafkide
g著Chi+mie st Physique Pho
tographiqua(Paul Mante1社刊
、 1967年)、 G、 F、 Duffin著Ph
otographic E+ulsion Chemi
stry (The FocalPress刊、 19
66年)、 v、 t、、 Zelikman et
al著Makingand CoatingPhoto
graphic Emulsion(The Foca
l Press刊−1964年)などに記載された方法
を用いて調整することができる。即ち、酸性法、中性法
、アンモニア法等のいずれでもよく。The photographic emulsion used in the present invention is P, Glafkide.
Written by gChi+mie st Physique Pho
tographiqua (Paul Mante 1, 1967), G. F. Duffin, Ph.
otographic E+ulsion Chemi
stry (The Focal Press, 19
66), v, t,, Zelikman et.
Makingand Coating Photo by al
Graphic Emulsion (The Foca
1 Press, 1964). That is, any of the acid method, neutral method, ammonia method, etc. may be used.
又可溶性銀塩と可溶性ハロゲン塩を反応させる形式とし
ては1片側混合法、同時混合法、それらの組合せなどの
いずれを用いてもよい。Further, as a method for reacting the soluble silver salt and the soluble halogen salt, any one-sided mixing method, simultaneous mixing method, or a combination thereof may be used.
粒子を銀イオン過剰の下において形成させる方法(いわ
ゆる逆混合法)を用いることもできる。同時混合法の一
つの形式としてハロゲン化銀の生成される液相中のPA
gを一定に保つ方法、即ち、いわゆるコンドロールド・
ダブルジェット法を用いることもできる。It is also possible to use a method in which particles are formed in an excess of silver ions (so-called back-mixing method). PA in the liquid phase in which silver halide is produced as a form of simultaneous mixing method
A method of keeping g constant, that is, a so-called chondral
A double jet method can also be used.
この方法によると、結晶形が規則的で粒子サイズが均一
に近いハロゲン化銀乳剤が得られる。According to this method, a silver halide emulsion having a regular crystal shape and a nearly uniform grain size can be obtained.
別々に形成した2種以上のハロゲン化銀乳剤を混合して
用いてもよい。Two or more types of silver halide emulsions formed separately may be mixed and used.
本発明に用いられるハロゲン化銀乳剤としては、公開技
報86−9598号に記載されているような外表面にミ
ラー指数(n n 1)(n≧2、nは自然数)で定義
され゛る結晶面を有するハロゲン化銀粒子が好ましく用
いられる。The silver halide emulsion used in the present invention has a mirror index (n n 1) (n≧2, n is a natural number) on the outer surface as described in Kokai Technical Report No. 86-9598. Silver halide grains having crystal faces are preferably used.
また、特開昭61−75337号に記載されているよう
な表面から内部に向って空洞の導退部を有するハロゲン
化銀乳剤も好ましく用いられる。このような比表面積の
大きいハロゲン化銀乳剤は特に色増感した場合に同一体
積の乳剤と比べて感度を出しやすいため本発明と組合せ
るとより有効である。Also preferably used is a silver halide emulsion having a hollow guide portion from the surface toward the inside, as described in JP-A-61-75337. Such a silver halide emulsion having a large specific surface area is more effective when combined with the present invention because it is easier to achieve sensitivity than an emulsion having the same volume, especially when color sensitized.
また、特開昭57−133540号、同58−1085
26号あるいは同59−162540号に記載されてい
るようなホスト粒子に組成の具なる銀塩をエピタキシャ
ル成長させた複合粒子を本発明に好ましく用いることが
できる。このような粒子は貰感硬調の写真性を示すため
本発明と組み合わせると好ましい。Also, JP-A-57-133540, JP-A No. 58-1085
Composite particles prepared by epitaxially growing a silver salt having a specific composition on a host particle as described in No. 26 or No. 59-162540 can be preferably used in the present invention. Such particles are preferable in combination with the present invention because they exhibit photographic properties with high contrast.
また、特開昭61−14630号および同60−122
935号に記載されているようなテトラザインデン存在
下で成長させたハロゲン化銀乳剤は沃化銀含有率が窩く
単分散性が優れて、いるため富感度で優れた粒状性を示
すため本発明に用いるハロゲン化銀乳剤として好ましく
用いられる。Also, JP-A-61-14630 and JP-A-60-122
The silver halide emulsion grown in the presence of tetrazaindene as described in No. 935 has excellent monodispersity with a low silver iodide content, and exhibits rich sensitivity and excellent graininess due to the presence of silver iodide. It is preferably used as a silver halide emulsion for use in the present invention.
また、特開昭58−126526号に示されるように。Also, as shown in Japanese Patent Application Laid-Open No. 58-126526.
含窒素複素環化合物の存在下で金硫貿増感も1シ<は金
セレン増感を行ったハロゲン化銀乳剤はかぶりが少なく
感度が高い性能を示すため1本発明に用いるハロゲン化
銀乳剤として好ましく用いられる。Silver halide emulsions that have undergone gold-sulfur sensitization in the presence of a nitrogen-containing heterocyclic compound are also used in the present invention because they exhibit low fog and high sensitivity. It is preferably used as
また、特開昭59−149345号あるいは同59−1
49344号に記載された。わずかに丸味を帯びた立方
体または14面体結晶は、高感度の性能が得られるため
本発明に用いられるハロゲン化銀乳剤として好ましい。Also, JP-A-59-149345 or JP-A No. 59-1
It was described in No. 49344. Slightly rounded cubic or tetradecahedral crystals are preferred as silver halide emulsions used in the present invention because they provide high sensitivity performance.
ハロゲン化銀粒子形成又は物理熟成の過程において、カ
ドミウム塩、亜鉛塩、鉛塩、タリウム塩。In the process of silver halide grain formation or physical ripening, cadmium salt, zinc salt, lead salt, thallium salt.
イリジウム塩又はその錯塩、ロジウム塩又はその錯塩、
鉄塩又はその錯塩などを、共存させてもよい。Iridium salt or its complex salt, rhodium salt or its complex salt,
Iron salts or complex salts thereof may also be present.
これらのうち、イリジウムの存在下で粒子形成されたハ
ロゲン化銀乳剤は高感度であるため(特公昭43−49
35号、特公昭45−32738号)、本発明に使用さ
れるハロゲン化銀乳剤として特に好ましい。Among these, silver halide emulsions in which grains are formed in the presence of iridium have high sensitivity (Japanese Patent Publication No. 43-49
No. 35, Japanese Patent Publication No. 45-32738) is particularly preferred as the silver halide emulsion used in the present invention.
乳剤は沈澱形成後あるいは物理熟成後に、通常可溶性塩
類を除去されるが、そのための手段、としては古くから
知られたゼラチンをゲル化させて行うターデル水洗法を
用いてもよく、また多価アニオンより成る無機塩類、例
えば硫酸ナトリウム。After the emulsion is precipitated or physically ripened, soluble salts are usually removed, and the long-known Tardel water washing method, which involves gelatinizing gelatin, may be used to remove polyvalent anions. Inorganic salts such as sodium sulfate.
アニオン性界面活性剤、アニオン性ポリマー(例えばポ
リスチレンスルホン酸)、あるいはゼラチン誘導体(例
えば脂肪族アシル化ゼラチン、芳香族アシル化ゼラチン
、芳香族カルバモイル化ゼラチンなど)を利用した沈降
法(フロキュレーション)を用いてもよい。Precipitation methods (flocculation) using anionic surfactants, anionic polymers (e.g. polystyrene sulfonic acid), or gelatin derivatives (e.g. aliphatic acylated gelatin, aromatic acylated gelatin, aromatic carbamoylated gelatin, etc.) may also be used.
ハロゲン化銀乳剤は1通常は化学増感される。Silver halide emulsions are usually chemically sensitized.
化学増感のためには9例えばH,Fr1essr4:
”DieGrundlagander Photogr
aphischen Prozessa witSil
bsr−halol(sniden” (Akadem
lscheVerlagsgesallchaft、
1968) 675−734頁に記載の方法を用いるこ
とができる。For chemical sensitization, 9 e.g. H, Fr1essr4:
”DieGrundlagander Photogr.
aphischen Prozessa witSil
bsr-halol (sniden) (Akadem
lscheVerlagsgesallchaft,
1968), pages 675-734, can be used.
すなわち、活性ゼラチンや銀と反応しうる硫黄を含む化
合物(例えば、チオ硫酸塩、チオ尿素類、メルカプト化
合物類、ローダニン類)を用いる硫黄増感法;還元性物
質(例えば、第一すず塩、アミン類、ヒドラジン誘導体
、ホルムアミジン区ルフィン酸、シラン化合物)を用い
る還元増感法;貴金属化合物(例えば、全錯塩のほかP
t+ xr、 Pdなどの周期律表■族の金属の錯塩)
を用いる責金焉増感法などを単独または組み合わせて用
いることができる。That is, sulfur sensitization using sulfur-containing compounds that can react with active gelatin and silver (e.g., thiosulfates, thioureas, mercapto compounds, rhodanines); reducing substances (e.g., stannous salts, Reduction sensitization method using noble metal compounds (e.g., total complex salts and P
Complex salts of metals from group II of the periodic table such as t+ xr and Pd)
A sensitization method using sensitization can be used alone or in combination.
また、活性ゼラチンや銀と反応しうるセレンを含む化合
物を用いるセレン増感法を他の増感法と組み合わせて用
いると高感度の乳剤が得られるので好ましい、この技術
は、米国特許第1,574,944号、第1,602,
592号、第1,623,499号、特公昭52−38
408号、特公昭57−22090号、特開昭59−1
80536号、米国特許第4,565,778号、特開
昭59−185329号、特開昭60−150046号
などに記述されている。Furthermore, it is preferable to use a selenium sensitization method using a selenium-containing compound that can react with active gelatin or silver in combination with other sensitization methods because a highly sensitive emulsion can be obtained.This technique is described in U.S. Pat. No. 574,944, No. 1,602,
No. 592, No. 1,623,499, Special Publication No. 52-38
No. 408, Japanese Patent Publication No. 57-22090, Japanese Patent Publication No. 59-1
No. 80536, US Pat. No. 4,565,778, Japanese Patent Application Laid-open No. 185329/1982, and Japanese Patent Application Laid-Open No. 150046/1984.
本発明に用いられる写真乳剤は、メチン色素類その他に
よって必要に応じて分光増感される3、用いられる色素
には、シアニン色素、メロシアニン色素、複合シアニン
色素、複合メロシアニン色素。The photographic emulsion used in the present invention is spectrally sensitized with methine dyes and others as necessary.3 Dyes used include cyanine dyes, merocyanine dyes, complex cyanine dyes, and complex merocyanine dyes.
ホロポーラ−シアニン色素、ヘミシアニン色素。Holopolar cyanine dye, hemicyanine dye.
スチリル°色素およびヘミオキソノール色素が包含され
る。特に有用な色素は、シアニン色素、メロシアニン色
素、および複合メロシアニン色素に属する色素である。Included are styryl° dyes and hemioxonol dyes. Particularly useful dyes are those belonging to the cyanine dyes, merocyanine dyes, and complex merocyanine dyes.
これらの色素類には、塩基性具B環核としてシアニン色
素類に通常利用される核のいずれをも適用できる。すな
わち、ピロリン核。Any of the nuclei commonly used for cyanine dyes can be used as the basic ring B ring nucleus for these dyes. i.e. pyrroline nucleus.
オキサゾリン核、チアゾリン核、ビロール核、オキサゾ
ール核、チアゾール核、セレナゾール核。Oxazoline nucleus, thiazoline nucleus, virol nucleus, oxazole nucleus, thiazole nucleus, selenazole nucleus.
イミダゾール核、テトラゾール核、ピリジン核など;こ
れらの核に脂環式炭化水素環が融合した核;及びこれら
の核に芳香族炭化水素環が融合した核。An imidazole nucleus, a tetrazole nucleus, a pyridine nucleus, etc.; a nucleus in which an alicyclic hydrocarbon ring is fused to these nuclei; and a nucleus in which an aromatic hydrocarbon ring is fused to these nuclei.
即チ、インドレニン核、ベンズインドレニン核。Sokuchi, indolenine nucleus, benzindolenine nucleus.
インドール核、ベンズオキサドール核、ナフトオキサゾ
ール核、ベンゾチアゾール核、ナフトチアゾール核、ベ
ンゾセレナゾール核、ベンズイミダゾール核、キノリン
核などが適用できる。これらの核は炭素原子上に置換さ
れていてもよい。Indole nucleus, benzoxadol nucleus, naphthoxazole nucleus, benzothiazole nucleus, naphthothiazole nucleus, benzoselenazole nucleus, benzimidazole nucleus, quinoline nucleus, etc. are applicable. These nuclei may be substituted on carbon atoms.
メロシアニン色素または複合メロシアニン色素にはケト
メチレン構造を有する核として、ピラゾリン−5−オン
核、チオヒダントイン核、2−チオオキサシリ゛ンジン
ー2,4−ジオン核、チアゾリジン−2゜4−ジオン核
、ローダニン核、チオバルビッール酸根などの5〜6員
異節環核を適用することができる。Merocyanine dyes or composite merocyanine dyes include a nucleus having a ketomethylene structure such as a pyrazolin-5-one nucleus, a thiohydantoin nucleus, a 2-thioxacyrindin-2,4-dione nucleus, a thiazolidine-2゜4-dione nucleus, a rhodanine nucleus, A 5- to 6-membered heteroartic ring nucleus such as a thiobarbyl acid radical can be applied.
有用な増感色素としては例えば、ドイツ特許929.0
80号、米国特許2,231,658号、同2,493
,748号、同2,503,776号、同2,519,
001号、同2,912,329号。Useful sensitizing dyes include, for example, German Patent No. 929.0
No. 80, U.S. Patent No. 2,231,658, U.S. Patent No. 2,493
, No. 748, No. 2,503,776, No. 2,519,
No. 001, No. 2,912,329.
同3,656,959号、同3,672,897号、同
3,694,217号。No. 3,656,959, No. 3,672,897, No. 3,694,217.
同4,025,349号、同4,046,572号、英
国特許1.242,588号、特公昭44−14030
号、同52−24844号に記載されたものを挙げるこ
とが出来る。No. 4,025,349, No. 4,046,572, British Patent No. 1.242,588, Japanese Patent Publication No. 44-14030
No. 52-24844.
これらの増感色素は単独に用いてもよいが、それらの組
合せを泪いてもよく、増感色素の組合せは特に9強色増
感の目的でしばしば用いられる。These sensitizing dyes may be used alone or in combination, and combinations of sensitizing dyes are often used particularly for the purpose of 9 supersensitization.
その代表例は米国特許2,688,545号、同2,9
77.229号、同3,397,060号、同3,52
2,052号。Typical examples are U.S. Pat. Nos. 2,688,545 and 2,9
No. 77.229, No. 3,397,060, No. 3,52
No. 2,052.
同3,527,641号、同3,617,293号、同
3,628,964号。No. 3,527,641, No. 3,617,293, No. 3,628,964.
同3,666.480号、同3,672,898号、同
3,679,428号。No. 3,666.480, No. 3,672,898, No. 3,679,428.
同3,703,377号、同3,769,301号、同
3,814,609号、同3,837,862号、同4
,026,707号、英国特許1.344,281号、
同1 、507 、1103号、特公昭43−4936
号、同53〜12375号、特開昭52−110618
号、同52−109925号に記載されている。No. 3,703,377, No. 3,769,301, No. 3,814,609, No. 3,837,862, No. 4
, No. 026,707, British Patent No. 1.344,281,
1, 507, No. 1103, Special Publication No. 43-4936
No. 53-12375, JP-A-52-110618
No. 52-109925.
増感色素とともに、それ自身分光増感作用をもたない色
素あるいは可視光を実質的に吸収しない物質であって、
強色増感を示す物質を乳剤中に含んでもよい1例えば、
含窒素異蹄環基で置換されたアミノスチル化合物)たと
えば米国特許2.933,390号、同3,635,7
21号に記載のもの)、芳香族有機酸ホルムアルデヒド
縮合物(たとえば米国特許3,743,510号に記載
のもの)、カドミウム塩、アザインデン化合物などを含
んでもよい、米国特許3,615,613号、同3,6
15,641号、同3,617,295号。Along with the sensitizing dye, it is a dye that itself does not have a spectral sensitizing effect or a substance that does not substantially absorb visible light,
The emulsion may contain a substance exhibiting supersensitization, for example,
Aminostyl compounds substituted with nitrogen-containing heterocyclic groups) For example, U.S. Pat.
No. 21), aromatic organic acid formaldehyde condensates (such as those described in U.S. Pat. No. 3,743,510), cadmium salts, azaindene compounds, etc., U.S. Pat. No. 3,615,613. , 3, 6
No. 15,641, No. 3,617,295.
同3,635,721号に記載の組合せは特に有用であ
る。The combination described in No. 3,635,721 is particularly useful.
本発明において用いられる漂白促進剤放出型化合物(以
下、BAR化合物という)は好ましくは下記一般弐N)
で表わされる。The bleach accelerator-releasing compound (hereinafter referred to as BAR compound) used in the present invention is preferably the following general 2N).
It is expressed as
一般式(+)
、A −(T+)t −(B −(h)、) ’、 −
2−S式(1)においてAは芳香族第一級アミン現像薬
の酸化体との反応により(T+)i以下との結合が開裂
する基を、T1及びT!はタイミング基を、Bは(T+
)z以上との結合が開裂した後芳香族第−級アミン現像
薬の酸化体との反応により(TりA以下との結合が開裂
する基を、Zは(B (T宜)−) −以上との結合
が開裂した後漂白促進作用を表わす基を、2、m及びn
は0またはlの整数を表わす。General formula (+), A −(T+)t −(B −(h),)′, −
In the 2-S formula (1), A is a group whose bond with (T+)i or less is cleaved by reaction with the oxidized product of an aromatic primary amine developer, and T1 and T! is the timing group, B is (T+
) After the bonds with Z and above are cleaved, by reaction with the oxidized product of the aromatic primary amine developer (T), Z is a group whose bonds with A and below are cleaved (B (T) -) - After the bond with the above is cleaved, groups exhibiting a bleaching accelerating effect are
represents an integer of 0 or l.
一般式(1)においてAは詳しくはカプラー残基または
還元剤残基を表わす。In general formula (1), A specifically represents a coupler residue or a reducing agent residue.
Aが表わすカプラー残基としては公知のものが使用でき
る0例えばイエローカプラー残基(例えば開鎖ケトメチ
レン型カプラー残基)、マゼンタカプラー残基(例えば
5−ピラゾロン型、ピラゾロイミダゾール型、ピラゾロ
トリアゾール型などのカプラー残基)、シアンカプラー
残基(例えばフェノール型、ナフトール型などのカプラ
ー残基)、および無呈色カプラー残基(例えばインダノ
ン型、アセトンフェノン型などのカプラー残基)が挙げ
られる。また、欧州特許第249453号、米国特許第
4,315,070号、同4.183.752号、同3
,961,959号または同4.171.223号に記
載のへテロ環型のカプラー残基であってもよい。As the coupler residue represented by A, known ones can be used.For example, yellow coupler residue (e.g., open-chain ketomethylene type coupler residue), magenta coupler residue (e.g., 5-pyrazolone type, pyrazoloimidazole type, pyrazolotriazole type) etc.), cyan coupler residues (eg, phenol type, naphthol type, etc. coupler residues), and colorless coupler residues (eg, indanone type, acetonephenone type, etc. coupler residues). Also, European Patent No. 249453, U.S. Patent No. 4,315,070, U.S. Patent No. 4.183.752, U.S. Patent No. 3
, 961,959 or 4.171.223.
一般式(1)においてAがカプラー残基を表わすときA
の好ましい例は下記一般式(Cp−1)、(C’p−2
)、(Cp−3)、(Cp−4)、(cp−s>、(C
p−6)、(Cp−7)、(Cp−8)、(Cp−9)
または(Cp−10)で表されるカプラー残基であると
きである。これらのカプラーはカップリング速度が大き
く好ましい。When A represents a coupler residue in general formula (1), A
Preferred examples of the following general formulas (Cp-1) and (C'p-2
), (Cp-3), (Cp-4), (cp-s>, (C
p-6), (Cp-7), (Cp-8), (Cp-9)
or (Cp-10). These couplers are preferred because of their high coupling speed.
一般式(Cp−1)
)(s+ シシtl シN M −KSz一般式(Cp
−2)
o 0
一般式(Cp−3)
一般式(Cp−4)
一般式(Cp−5)
一般式(Cp−6)
H
一般式(Cp−7)
(”II
一般式(Cp−8)
O■
一般式(Cp−9)
一般式(Cp−10)
上式においてカップリング位より派生している自由結合
手は、カップリング離脱基の結合位置を表わす。General formula (Cp-1) )(s+
-2) o 0 General formula (Cp-3) General formula (Cp-4) General formula (Cp-5) General formula (Cp-6) H General formula (Cp-7) ("II General formula (Cp-8 ) O■ General formula (Cp-9) General formula (Cp-10) In the above formula, the free bond derived from the coupling position represents the bonding position of the coupling-off group.
上式においてR8I、Rs!、R5I、RlJ、R%%
、R’S4、R5ff、Rs、、R%9、Ra。、Ra
+5RizまたはR43が耐拡散基を含む場合、それは
炭素数の総数が8ないし40、好ましくは10ないし3
0になるように選択され、それ以外の場合、炭素数の総
数は15以下が好ましい、ビス型、テロマー型またはポ
リマー型のカプラーの場合には上記の置換基のいずれか
が二価基を表わし、繰り返し単位などを連結する。この
場合には炭素数の範囲は規定外であってもよい。In the above formula, R8I, Rs! , R5I, RlJ, R%%
, R'S4, R5ff, Rs, , R%9, Ra. , Ra
When +5Riz or R43 contains a diffusion-resistant group, it has a total number of carbon atoms of 8 to 40, preferably 10 to 3.
0, otherwise the total number of carbon atoms is preferably 15 or less; in the case of bis-, telomeric- or polymeric couplers, any of the above substituents represents a divalent group; , concatenate repeating units, etc. In this case, the range of carbon numbers may be outside the specified range.
以下にRsI〜R1、dおよびeについて詳しく説明す
る。以下でRatは脂肪族基、芳香族基または複素環基
を表わし、R4zは芳香族基または複素環基を表わし、
R42SR4AおよびRd%は水素原子、脂肪族基、芳
香族基または複素環基を表わす。RsI to R1, d and e will be explained in detail below. In the following, Rat represents an aliphatic group, an aromatic group or a heterocyclic group, R4z represents an aromatic group or a heterocyclic group,
R42SR4A and Rd% represent a hydrogen atom, an aliphatic group, an aromatic group or a heterocyclic group.
R’SIはR41と同じ意味を表わすeR%!およびR
s、は各々R4tと同じ意味を表わす、R34はR11
と同じ意味の基、R,、C0N−基、R4,N−基、R
Ajl に
RssはR41と同じ意味の基を表わす*R%hおよび
RS?は各々Ray基と同じ意味の基、R4+S−基、
R4,〇−基、R,、C0N−基、R4コ
またはR,,5O1N−基を表わす*R8IはRn1と
Rn3
同じ意味の基を表わす、R3,はRatと同じ意味のR
4,〇−基、R,、S−基、ハロゲン原子、またはRa
+N−5を表わす、dはOないし3を表わす。R'SI is eR% which has the same meaning as R41! and R
s, each has the same meaning as R4t, R34 is R11
A group having the same meaning as R,, C0N- group, R4, N- group, R
Rss in Ajl represents a group with the same meaning as R41 *R%h and RS? are each a group having the same meaning as Ray group, R4+S- group,
R4, represents a group with the same meaning as Rn1 and Rn3, R3 represents an R group with the same meaning as Rat
4,0- group, R,, S- group, halogen atom, or Ra
+N-5; d represents O to 3;
■
dが複数のとき複数個のR%Qは同じ置換基または異な
る置換基を表わす、またそれぞれのR59が2価基とな
って連結し環状構造を形成してもよい。(2) When d is a plurality of R%Qs, the plurality of R%Qs represent the same substituent or different substituents, and each R59 may become a divalent group and connect to form a cyclic structure.
環状構造を形成するための2価基の例としてはが代表的
な例として挙げられる。ここでfは0ないし4の整数、
gはOないし2の整数、を各々表わす、R6゜はRoと
同じ意味の基を表わす。R61はR41と同じ意味の基
、RbzはR41と同じ意味の基、R,、C0NH−基
、
R,,0CONH−基、R,、SO□NH−基、R,,
0−基、R□s−4、ハロゲン原子またはR,、N−基
を表わす、R&3はRa 1と同し意味の基、R,,5
Offi−基、R,,0CO−基、R,,0−3o!−
基、ハロゲン原子、ニド四基、シアノ基またはR,3C
O−基を表わす、eは0ないし4の整数を表わす、複数
個のRbtまたはR63があるとき各々同じものまたは
異なるものを表わす。Typical examples of divalent groups for forming a cyclic structure include: Here f is an integer from 0 to 4,
g represents an integer from O to 2, and R6° represents a group having the same meaning as Ro. R61 is a group with the same meaning as R41, Rbz is a group with the same meaning as R41, R,, C0NH- group, R,,0CONH- group, R,, SO□NH- group, R,,
0- group, R□s-4, represents a halogen atom or R,,N- group, R&3 is a group having the same meaning as Ra 1, R,,5
Offi- group, R,,0CO- group, R,,0-3o! −
group, halogen atom, nido tetragroup, cyano group or R, 3C
represents an O- group, e represents an integer from 0 to 4, and when there is a plurality of Rbt or R63, each represents the same or different.
上記において脂肪族基とは炭素数1〜32、好ましくは
1〜22の飽和または不飽和、鎖状または環状、直鎖ま
たは分岐、置換または無置換の脂肪族炭化水素基である
。代表的な例としては、メチル、エチル、プロピル、イ
ソプロピル、ブチル、(1)−ブチル、(+)−ブチル
、(1)−7ミル、ヘキシル、シクロヘキシル、2−エ
チルへキシル、オクチル、1.1,3.3−テトラメチ
ルブチル、デシル、ドデシル、ヘキサデシル、またはオ
クタデシルが挙げられる。In the above, the aliphatic group is a saturated or unsaturated, chain or cyclic, straight chain or branched, substituted or unsubstituted aliphatic hydrocarbon group having 1 to 32 carbon atoms, preferably 1 to 22 carbon atoms. Representative examples include methyl, ethyl, propyl, isopropyl, butyl, (1)-butyl, (+)-butyl, (1)-7mil, hexyl, cyclohexyl, 2-ethylhexyl, octyl, 1. Mention may be made of 1,3.3-tetramethylbutyl, decyl, dodecyl, hexadecyl, or octadecyl.
芳香族基とは炭素数6〜20好ましくは置換もしくは無
置換のフェニル基、または置換もしくは無置換のナフチ
ル基である。The aromatic group is preferably a substituted or unsubstituted phenyl group having 6 to 20 carbon atoms, or a substituted or unsubstituted naphthyl group.
複素環基とは炭素数1〜20、好ましくは1〜7の、複
素原子として窒素原子、酸素原子もしくはイ゛オウ原子
から選ばれる、好ましくは3異ないし8員環の置換もし
くは無置換の複素環基である。A heterocyclic group is a substituted or unsubstituted heterocyclic group having 1 to 20 carbon atoms, preferably 1 to 7 carbon atoms, preferably a 3- to 8-membered ring selected from a nitrogen atom, an oxygen atom, or a sulfur atom. It is a ring group.
複素環基の代表的な例としては2−ピリジル、2−チエ
ニル、2−フリル、I−イミダゾリル、l−インドリル
、フタルイミド、1.3.4−チアジアゾール−2−イ
ル、2−キノリル、2.4−ジオキソ−1,3−イミダ
ゾリジン−5−イル、2.4−ジオキソ−1,3−イミ
ダゾリジン−3−イル、スクシンイミド、1.2.4−
トリアゾール−2−イルまたは1−ピラゾリルが挙げら
れる。Representative examples of the heterocyclic group include 2-pyridyl, 2-thienyl, 2-furyl, I-imidazolyl, l-indolyl, phthalimide, 1.3.4-thiadiazol-2-yl, 2-quinolyl, 2. 4-dioxo-1,3-imidazolidin-5-yl, 2,4-dioxo-1,3-imidazolidin-3-yl, succinimide, 1.2.4-
Mention may be made of triazol-2-yl or 1-pyrazolyl.
前記脂肪族炭化水素基、芳香族基および複素環基が置換
基を有するとき代表的な置換基としては、ハロケン原子
、R,、O−基、R−bs−基、K4@
バ4−
R,−NSOx−基、R,,5O1−、l、ぎ
R4嘗
R−’ToSOx−基、シアノ基またはニトロ基が挙げ
られる。ここでR46は脂肪族基、芳香族基、または複
素環基を表わし、Raq、RamおよびRaqは各々脂
肪族基、芳香族基、複素i基または水素原子を表わす、
脂肪族基、芳香族基または複素環基の意味は前に定義し
たのと同じ意味である。When the aliphatic hydrocarbon group, aromatic group and heterocyclic group have a substituent, typical substituents include a halogen atom, R,, O- group, R-bs- group, K4@
Examples include a R, -NSOx- group, a R,,5O1-, l, a R4R-'ToSOx- group, a cyano group or a nitro group. Here, R46 represents an aliphatic group, an aromatic group, or a heterocyclic group, and Raq, Ram, and Raq each represent an aliphatic group, an aromatic group, a hetero i group, or a hydrogen atom,
Aliphatic, aromatic or heterocyclic have the same meanings as defined above.
−a式(Cp−1)で表わされるカプラー残基は例えば
米国特許第3,933,501号、同第4゜022.6
20号、同第4,326.024号、同第4,401,
752号、特公昭5B−10739号、英国特許筒1,
425,020号、同第1.476.760号、同第2
49,473号等に具体的に記載されている。The coupler residue represented by the formula (Cp-1) is described, for example, in U.S. Patent Nos. 3,933,501 and 4°022.6.
No. 20, No. 4,326.024, No. 4,401,
No. 752, Special Publication No. 5B-10739, British Patent No. 1,
No. 425,020, No. 1.476.760, No. 2
It is specifically described in No. 49,473, etc.
一般式(Cp−2)で表わされるカプラー残基は例えば
米国特許第4,149,886号、英国特許1.204
,680号、特開昭52−154631号等に具体的に
記載されている。The coupler residue represented by the general formula (Cp-2) is disclosed in, for example, US Pat. No. 4,149,886, British Patent No. 1.204.
, No. 680, JP-A-52-154631, etc.
−M式(Cp−3)で表わされるカプラー残基は例えば
特開昭49−111631号、同54−48540号、
同55−62454号、同55−118034号、同5
6−38045号、同56−80045号、同56−1
26833号、同57−4044号、同57−3585
8号、同57−94752号、同5B−17440号、
同58−50537号、同58−85432号、同58
−117546号、同5B−126530号、同58−
145944号、同5B−205151号、特開昭54
−170号、同54−10491号、同54−2125
8号、同53−4E;452号、同53−46453号
、同57−36577号、特願昭58−110596号
、同58−132134号、同59−26729号、米
国特許3.227.554号、同第3,432,521
号、同第4.310,618号、同第4.351,89
7号等に具体的に記載されている。-M formula (Cp-3) is a coupler residue represented by, for example, JP-A-49-111631, JP-A-54-48540;
No. 55-62454, No. 55-118034, No. 5
No. 6-38045, No. 56-80045, No. 56-1
No. 26833, No. 57-4044, No. 57-3585
No. 8, No. 57-94752, No. 5B-17440,
No. 58-50537, No. 58-85432, No. 58
-117546, 5B-126530, 58-
No. 145944, No. 5B-205151, Japanese Unexamined Patent Publication No. 1973
-170, 54-10491, 54-2125
No. 8, No. 53-4E; No. 452, No. 53-46453, No. 57-36577, Japanese Patent Application No. 58-110596, No. 58-132134, No. 59-26729, U.S. Patent No. 3.227.554 No. 3,432,521
No. 4.310,618, No. 4.351,89
It is specifically described in No. 7, etc.
一般式(Cp−4)及び(CD−5)で表わされるカプ
ラー残基は例えば国際特許公開WO36101915号
、同86102467号、欧州特許公開(EP)182
617号、米国特許第3,061゜432号、同3,7
05,896号、同3.72j、 ’067号、同4,
500,630号、同4゜5’40,654号、同4.
548,899号、同4.581,326号、同4,6
07,002号、同4,621,046号、同4,67
5,280号、特開昭59−228252号、同60−
33552号、同60−43659号、同60−553
43号、同60−57838号、同60−98434号
、同60−107032号、同61−53644号、同
61−65243号、同61−65245号、同61−
65246号、同61−65247号、同61−120
146号、同61−120147号、同61−1201
48号、同61−120149号、同61−12015
0号。Coupler residues represented by general formulas (Cp-4) and (CD-5) are, for example, International Patent Publication No. WO36101915, International Patent Publication No. 86102467, European Patent Publication (EP) 182
No. 617, U.S. Patent No. 3,061°432, U.S. Patent No. 3,7
No. 05,896, No. 3.72j, No. 067, No. 4,
No. 500,630, No. 4゜5'40,654, No. 4.
No. 548,899, No. 4.581,326, No. 4.6
No. 07,002, No. 4,621,046, No. 4,67
No. 5,280, JP-A-59-228252, JP-A No. 60-
No. 33552, No. 60-43659, No. 60-553
No. 43, No. 60-57838, No. 60-98434, No. 60-107032, No. 61-53644, No. 61-65243, No. 61-65245, No. 61-
No. 65246, No. 61-65247, No. 61-120
No. 146, No. 61-120147, No. 61-1201
No. 48, No. 61-120149, No. 61-12015
No. 0.
同61−120151号、同61−120152号、同
61−120153号、同61−120154号、同6
1−141446号、同61−144647号、同61
−147254号、同61−151648号、同61−
180243号、同61−228444号、同61−2
30146号、同61−230147号、同61−29
2143号等に具体的に記載されている。No. 61-120151, No. 61-120152, No. 61-120153, No. 61-120154, No. 6
No. 1-141446, No. 61-144647, No. 61
-147254, 61-151648, 61-
No. 180243, No. 61-228444, No. 61-2
No. 30146, No. 61-230147, No. 61-29
It is specifically described in No. 2143 and the like.
一般式(Cp−6)、(Cp−7)及び(Cp−8)で
表されるカプラー残基は例えば米国特許第4,052゜
212号、同第4,146.396号、同第4゜228
.233号、同第4,296,200号、同第2.36
9,929号、同第2,801.171号、同第2,7
72,162号、同第2.895.826号、同第3.
772,002号、同第3,758,308号、同第4
.・334,011号、同第4,327,173号、西
独特許公開第3.329.729号、欧州特許第121
,365A号、米国特許第3,446,622号、同第
4,333,999号、同第4.451,559号、同
第4,427,767号、同第4,554.244号、
欧州特許第161,626A号、同175,573号、
同250,201号等に具体的に記載されている。Coupler residues represented by the general formulas (Cp-6), (Cp-7) and (Cp-8) are described, for example, in U.S. Pat.゜228
.. No. 233, No. 4,296,200, No. 2.36
No. 9,929, No. 2,801.171, No. 2,7
No. 72,162, No. 2.895.826, No. 3.
No. 772,002, No. 3,758,308, No. 4
..・No. 334,011, No. 4,327,173, West German Patent Publication No. 3.329.729, European Patent No. 121
, 365A, U.S. Patent Nos. 3,446,622, 4,333,999, 4.451,559, 4,427,767, 4,554.244,
European Patent No. 161,626A, European Patent No. 175,573,
It is specifically described in Nos. 250, 201 and the like.
一般式(Cp−9)で表わされるカプラー71!L基は
例えば米国特許第3,932,185号、同第4゜06
3.950号等に具体的に記載されてかる。Coupler 71 represented by general formula (Cp-9)! The L group is described, for example, in U.S. Pat. No. 3,932,185, U.S. Pat.
It is specifically described in No. 3.950, etc.
−“般式(Cp−10)で表わされるカプラー残基は例
えば米国特許第4,429,035号等に具体的に記載
されている。-"The coupler residue represented by the general formula (Cp-10) is specifically described in, for example, US Pat. No. 4,429,035.
一般式(Cp−1)で表わされるカプラー残基の典型例
が特願昭62−226050号における化合物例(Y−
1)〜(Y−34)により開示されており、同様に一般
式(Cp−3)で表わされるカプラー残基については化
合物例(M−1)〜(M−56) −により、一般
式(Cp−4)及び(Cp−5)で表わされるカプラー
残基については化合物例(M−57)〜(M−108)
により、一般式(Cp−6)及び(cp−7)で表わさ
れるカプラー残基については化合物例(C−1)〜(C
−56)により、一般式(Cp−13)で表されるカプ
ラー残基については化合物例(C−57)〜(C−86
)によりそれぞれその典型例が開示されている。A typical example of the coupler residue represented by the general formula (Cp-1) is the compound example (Y-
1) to (Y-34) and similarly represented by general formula (Cp-3), compound examples (M-1) to (M-56) - disclose general formula ( For coupler residues represented by Cp-4) and (Cp-5), compound examples (M-57) to (M-108)
Accordingly, for the coupler residues represented by general formulas (Cp-6) and (cp-7), compound examples (C-1) to (C
-56), for the coupler residue represented by the general formula (Cp-13), compound examples (C-57) to (C-86
) disclose their typical examples.
一般式(1)で表わされる化合物はZ以外の部分(好ま
しくはA)において互いに結合する二量体ないしポリマ
ー状の化合物であってもよく、その具体例は例えば特願
昭62−90442号に記載されている。The compound represented by the general formula (1) may be a dimeric or polymeric compound that is bonded to each other at a portion other than Z (preferably A), and specific examples thereof can be found, for example, in Japanese Patent Application No. 62-90442. Are listed.
Aが表わす還元剤残基としては、例えば特願昭62−2
03997号の第78頁一般式(I[)から第85頁一
般式(TV)により表わされる還元剤残基(例えばハイ
ドロキノン、ナフトハイドロキノン、カテコール、ピロ
ガロール、アミノフェノール、没食子酸等の誘導体の構
造を持つ残基)が−船釣である。As the reducing agent residue represented by A, for example, Japanese Patent Application No. 62-2
No. 03997, page 78 general formula (I[) to page 85 general formula (TV) (residues with) is - boat fishing.
一般式(1)においてT、及びT2で表わされるタイミ
ング基は種りの目的(例えばカップリング活性の調節)
で適宜用いられる。これらタイミング基の例として特願
昭62−186939号の第23頁から第36頁にかけ
ての項目(1)〜(5)及び(7)テ示されたものがあ
るが、これらの中では一瓜式(T−1)、(T−2)及
び(T−3)で表わされるタイミング基が好ましい。In general formula (1), the timing groups represented by T and T2 have various purposes (for example, regulation of coupling activity).
Used as appropriate. As examples of these timing groups, there are those shown in items (1) to (5) and (7) on pages 23 to 36 of Japanese Patent Application No. 186939/1980, but among these, only one Timing groups represented by formulas (T-1), (T-2) and (T-3) are preferred.
一瓜弐N)においてBで表される基は(T+)z以上の
基すなわち丁、またはAより離脱して後カプラーまたは
還元剤(例えばハイドロキノン、ナフトハイドロキノン
、カテコール、ピロガロール、アミノフェノール、没食
子酸等の誘導体)として機能し、カップリング反応また
は酸化還元反応によりT、以下を放出する基を表わす。The group represented by B in (T+)z or more in (T+)z or more, or a coupler or reducing agent (e.g. hydroquinone, naphthohydroquinone, catechol, pyrogallol, aminophenol, gallic acid) after detachment from A T represents a group that functions as a derivative (e.g., T) and releases the following by a coupling reaction or redox reaction.
例えば米国特許第4438193号、同第461857
1号9.特開昭60−203943号、同60−213
944号及び同61−236551号等に記載があり、
具体例として以下のような基が挙げられる。For example, US Pat. No. 4,438,193, US Pat. No. 4,618,57
No. 1 9. JP-A-60-203943, JP-A No. 60-213
There is a description in No. 944 and No. 61-236551, etc.
Specific examples include the following groups.
o−*
ここで*はT、との結合位!を、本章はT2との結合位
置をそれぞれ表わす。o-* Here * is the bonding position with T! This chapter shows the bonding position with T2.
↑1、T2及びBは目的に応じて適宜利用されるが、用
いない方が一般的に好ましい。↑1, T2 and B are used as appropriate depending on the purpose, but it is generally preferable not to use them.
一般式(1)においてZで表わされる基は詳しくは公知
の漂白促進剤残基が挙げられる0例えば米国特許第3.
893,858号明細書、英国特許第1138842号
明細書、特開昭53−141623号公報に記載されて
いる如き種々のメルカプト化合物、特開昭53−956
30号公報に記載されている如きジスルフィド結合を有
する化合物、特公昭53−9854号公報に記載されて
いる如きチアゾリジン誘導体、特開昭53〜94927
号公報に記載されている如きイソチオ尿素誘導体、特公
昭45−8506号公報、特公昭49−26586号公
報に記載されている如きチオ尿素誘導体、特開昭49−
42349号公報に記載されている如きチオアミド化合
物、特開昭55−26506号公報に記載されている如
きジチオカルバミン酸塩類、米国特許第4552834
号明細書に記載されている如きアリーレンジアミン化合
物等である。これらの化合物は、分子中に含まれる置換
可能なヘテロ原子において、−i式(1)におけるA−
(T+)t−CB−(T、)+1) 、−に結合するの
が好ましい例である。In the general formula (1), the group represented by Z is specifically a known bleach accelerator residue. For example, US Pat.
893,858, British Patent No. 1138842, JP-A-53-141623, JP-A-53-956;
Compounds having a disulfide bond as described in Japanese Patent Publication No. 30, thiazolidine derivatives as described in Japanese Patent Publication No. 53-9854, Japanese Patent Publication No. 53-94927
isothiourea derivatives as described in Japanese Patent Publication No. 45-8506, thiourea derivatives as described in Japanese Patent Publication No. 49-26586, Japanese Patent Publication No. 49-26586;
Thioamide compounds as described in JP-A-42349, dithiocarbamates as described in JP-A-55-26506, US Pat. No. 4,552,834
These include arylene diamine compounds as described in the specification of No. These compounds have -i in formula (1) A- in the substitutable heteroatom contained in the molecule.
A preferred example is bonding to (T+)t-CB-(T,)+1), -.
Zで表わされる基はさらに好ましくは下記−瓜式(Z−
1)、(Z−2)、(Z−3)、(Z−4)または(Z
−5)で表わされる。The group represented by Z is more preferably represented by the following formula (Z-
1), (Z-2), (Z-3), (Z-4) or (Z
−5).
一般式(Z−1) −3−L、−(χ1)。General formula (Z-1) −3−L, −(χ1).
一般式(Z−1)においてaは1〜4の整数を、し、は
a+1価の炭素原子数1〜8の直鎖状または分岐鎖状の
アルキレン基を、Xlはヒドロキシル基、カルボキシル
基、シアノ基、炭素原子数0〜10のアミノ基(例えば
アミノ、メチルアミノ、エチルアミノ、ジメチルアミノ
、ジエチルアミノ、ジイソプロピルアミン、ピロリン、
)、ピペリジノ、モルホリノ、ヒドロキソアミノ)、炭
素原子数1〜10のアシル基(例えばホルミル、アセチ
ル)、炭素原子数1〜1oのカルバモイル基(例えばカ
ルバモイル、ジメチルカルバモイル、ヒドロキンカルバ
モイル、モルホリノカルボニル)、炭素原子II〜10
のスルホニル基(例えばメチルスルホニル、エチルスル
ホニル)、炭素i子no〜10・のスルファモイル基(
例えばスルファモイル、メチルスルファモイル、ジメチ
ルスルファモイル、ピロリジノスルホニル)、炭素原子
数1〜10のカルボンアミド基(例えばホルムアミド、
アセトアミド)、炭素原子数3〜12のアンモニラミル
基(例えばトリメチルアンモニラミル、ピリジニラミル
)、炭素原子数1〜10のウレイド基(例えばウレイド
、3−メチルウレイド)、炭素原子数0〜10のスルフ
ァモイルアミノ基(例えばスルファモイルアミノ、3.
3−ジメチルスルファモイルアミノ)、炭素原子数1〜
6のアルコシ基(例えばメトキシ)、アミジノ基、グア
ジニノ基またはアミジノチオ基等をそれぞれ表わす、た
だしaが複数のとき複数のχ1は同しでも異なっていて
もよい、またL+はシクロアルキレン基であることはな
く、具体例としてメチレン、エチレン、ト、リメチレン
、エチリデン、イソプロピリデン、プロピレン、1,2
.3−プロパントリイル等力ある。In the general formula (Z-1), a is an integer of 1 to 4, a+ is a monovalent linear or branched alkylene group having 1 to 8 carbon atoms, Xl is a hydroxyl group, a carboxyl group, Cyano group, amino group having 0 to 10 carbon atoms (e.g. amino, methylamino, ethylamino, dimethylamino, diethylamino, diisopropylamine, pyrroline,
), piperidino, morpholino, hydroxoamino), acyl groups having 1 to 10 carbon atoms (e.g. formyl, acetyl), carbamoyl groups having 1 to 1 o carbon atoms (e.g. carbamoyl, dimethylcarbamoyl, hydroquinecarbamoyl, morpholinocarbonyl), Carbon atoms II-10
sulfonyl group (e.g. methylsulfonyl, ethylsulfonyl), sulfamoyl group with carbon atoms no. to 10.
For example, sulfamoyl, methylsulfamoyl, dimethylsulfamoyl, pyrrolidinosulfonyl), carbonamide groups having 1 to 10 carbon atoms (for example, formamide,
acetamide), ammoniayl group having 3 to 12 carbon atoms (e.g. trimethylammonillamyl, pyridinylamyl), ureido group having 1 to 10 carbon atoms (e.g. ureido, 3-methylureido), sulfamoyl group having 0 to 10 carbon atoms Amino groups (e.g. sulfamoylamino, 3.
3-dimethylsulfamoylamino), carbon number 1 -
6 each represents an alkoxy group (e.g. methoxy), amidino group, guazinino group, or amidinothio group, etc., provided that when a is plural, the plural χ1s may be the same or different, and L+ is a cycloalkylene group Specific examples include methylene, ethylene, t, rimethylene, ethylidene, isopropylidene, propylene, 1,2
.. 3-Propanetriyl etc.
一般式(Z−2)
一般式(Z−2)においてbは1〜6の整数を、Cは0
〜7の整数を、Lx及びり、は炭素原子数1〜3の直鎖
状または分岐鎖状のアルキレン基を、Xl及びX、は一
般式(Z−1)におけるX、と同じ意味を、Ylは一〇
−1−S−1−SO−1−CO−1−NSO,N−1−
3O,N−1R+ Rz R。General formula (Z-2) In general formula (Z-2), b is an integer from 1 to 6, and C is 0.
An integer of ~7, Lx and R represent a linear or branched alkylene group having 1 to 3 carbon atoms, Xl and X have the same meaning as X in general formula (Z-1), Yl is 10-1-S-1-SO-1-CO-1-NSO, N-1-
3O, N-1R+ Rz R.
−COO−2−OCO−1−OCO〇−1−〇C0N−
1−NC0○−または−NSO,−R1RI
R。-COO-2-OCO-1-OCO〇-1-〇C0N-
1-NC0○- or -NSO, -R1RI
R.
(ただしR,及びR1は水素原子または炭素原子数1〜
10のアルキル基(例えばメチル、エチル、ヒドロキシ
メチル、ヒドロキシエチル、メトキノエチル、カルボキ
シメチル、カルボキシエチル、プロピル等を表わす、)
をそれぞれ表わす、ただし、bが複数のとき複数のY
l−L sは同しでも異なっ、ていてもよい(ただし、
すべてのY、が−S−であることはない、)また、Cが
0以外のときX2は置換可能な場合Lz 、Y、 、+
3のいずれにも置換することができる。(However, R and R1 are hydrogen atoms or have 1 to 1 carbon atoms.
10 alkyl groups (representing, for example, methyl, ethyl, hydroxymethyl, hydroxyethyl, methquinoethyl, carboxymethyl, carboxyethyl, propyl, etc.)
respectively, but when b is plural, plural Y
l-L s may be the same or different (but
(Not all Y, is -S-) Also, when C is non-zero, X2 is substitutable Lz, Y, , +
Any of 3 can be substituted.
一般式(Z−3)
一般式(Z−3)において、bSc、Lx 、+3、χ
、及びX、は一般式(Z−2)におけるす、c、Lx
、+3 、Xl及びX!とそれぞれ同じ意味を、Wは−
0−1−S−1−〇〇〇−1−0S O!−1Kコ
1<コそれぞれ表わす。こ
こでR5は一般式(Z 2)におけるR1 と同じ意
味を、R4はR2と同じ宥味を、WIは一〇−1−〇〇
〇−−〇SO,−1−OSO−または−N−をそれぞれ
表わす、またRコ
bが複数のとき、複数のS−L、は同じでも異なってい
てもよく、Cが0以外のときX2はHA可能な場合W、
L2及びり、のいずれにも置換することができる。ただ
し、Wが−S−であるときbは1であることはない。General formula (Z-3) In general formula (Z-3), bSc, Lx, +3, χ
, and X are Su, c, and Lx in general formula (Z-2)
, +3, Xl and X! and W has the same meaning respectively, and -
0-1-S-1-〇〇〇-1-0S O! -1K
1<K represents each. Here, R5 has the same meaning as R1 in general formula (Z2), R4 has the same palatability as R2, and WI is 10-1-000--0SO, -1-OSO- or -N- respectively, and when Rcob is multiple, multiple S-L may be the same or different, and when C is other than 0, X2 is W if HA is possible,
It can be replaced with either L2 or . However, b is never 1 when W is -S-.
一般式(Z−4)
一般式(Z−4)においてW1χ1及びX!は一般式(
Z−3)におけるW2χ、及びX2とそれぞれ同じ意味
をdはO〜6の整数を、R4及びり、は総炭素原子数1
〜16の連結基(例えばアルキレンや一〇−1−S−1
−N−で互いに結合するアルキレン)をそれぞれ表わす
。ただしR4は一般式(Z−2)におけるR8と同じ意
味を表わし、dがO以外のときχ2は置換可能な場合V
J、R4及びLsのいずれにも置換することができる。General formula (Z-4) In general formula (Z-4), W1χ1 and X! is the general formula (
Z-3) has the same meaning as W2χ and
~16 linking groups (e.g. alkylene, 10-1-S-1
-N- represents alkylene bonded to each other. However, R4 has the same meaning as R8 in general formula (Z-2), and when d is other than O, χ2 is V when it is substitutable.
Any of J, R4 and Ls can be substituted.
一般式(Z−5) −5−LA −(X3)。General formula (Z-5) -5-LA-(X3).
一般式(Z−5)においてR6は炭素原子数3〜12の
シクロヘキサンル基(例えばシクロプロパン、シクロブ
タン、シクロベンクン、メチルシクロベンクン、シクロ
ヘキサン、シクロブンタノジ、シクロヘキサノン、ビシ
クロ(2,2,1)ペンタン等から誘導される基)、炭
素原子数6〜10のアリーレン基(例えばフェニレン、
ナフチレン)、炭素原子数1〜10の不飽和複素環基(
例えばビロール、ピラゾール、イミダソール、1.2.
3−トリアゾール、1,2.4−トリアゾール、テトラ
ゾール、オキサゾール、チアゾール、インドール、イン
ダゾール、ベンズイミダゾール、ベンゾオキサゾール、
ベンゾチアゾール、1.3.4−オキサシアプール、1
.3.4−チアジアゾール、プリン、テトラアザインデ
ン、イソオキサゾール、イソチアゾール、ピリジン、ピ
リミジン、とリダジン、1.3.5−トリアジン、キノ
リン、フラン、チオフェン等から誘導される基)または
炭素原子数2〜10の部分的に飽和であってもよい飽和
複素環基(例えばオキシラン、チイラン、アジリジン、
オキセタン、オキソラン、チオラン、チエクン、オキサ
ン、チアン、ジチオン、ジオキサン、ピペリジン、モル
ホリン、ピペラジン、イミダゾリジン、ピロリジン、ピ
ラゾリン、ピラゾリジン、イミダシリン、ピラン、チオ
ビラン、オキサゾリン、スルホラン等から誘導される基
)を表わす。In general formula (Z-5), R6 is a cyclohexane group having 3 to 12 carbon atoms (e.g., cyclopropane, cyclobutane, cyclobencune, methylcyclobencune, cyclohexane, cyclobuntanodi, cyclohexanone, bicyclo(2,2,1)pentane, etc. ), arylene groups having 6 to 10 carbon atoms (e.g. phenylene,
naphthylene), unsaturated heterocyclic groups having 1 to 10 carbon atoms (
For example virol, pyrazole, imidasol, 1.2.
3-triazole, 1,2.4-triazole, tetrazole, oxazole, thiazole, indole, indazole, benzimidazole, benzoxazole,
Benzothiazole, 1.3.4-oxacyapur, 1
.. 3.4-thiadiazole, purine, tetraazaindene, isoxazole, isothiazole, pyridine, pyrimidine, ridazine, 1.3.5-triazine, quinoline, furan, thiophene, etc.) or a group having 2 carbon atoms ~10 optionally partially saturated saturated heterocyclic groups (e.g. oxirane, thiirane, aziridine,
represents a group derived from oxetane, oxolane, thiolane, thiecune, oxane, thiane, dithione, dioxane, piperidine, morpholine, piperazine, imidazolidine, pyrrolidine, pyrazoline, pyrazolidine, imidacilline, pyran, thiovilane, oxazoline, sulfolane, etc.
一般式(Z〜5)においてX2は親水性置換基を表わし
、好ましくはπttA基定数で0.5以下、さらに好ま
しくは負の値となる置換基である。π置換基定数とは“
サブスティテユエント・コンスタント・フォア・コリレ
ーシヨン・アナリシス・イン・ケミストリー・アンド・
バイオロジー(5ubstituent Con5ta
nts for CorrelationAnalys
is in Chemistry and Biolo
gy ) 、C,ハンシュ(C,Hansch)および
A、レオ(^ルeo)著、ジョン・ウィリー(John
Wiley) 1979年に記載の方法により、X
、について計算される値である。In the general formulas (Z to 5), X2 represents a hydrophilic substituent, preferably a substituent having a πttA group constant of 0.5 or less, more preferably a negative value. What is π substituent constant?
Substitute Constant for Correlation Analysis in Chemistry and
Biology (5ubstituent Con5ta)
nts for CorrelationAnalyses
is in Chemistry and Biolo
gy ), C. Hansch and A. leo, John Wiley.
Wiley) by the method described in 1979,
, is the value calculated for .
例えば下記のものが挙げられる。()内にπ置換基定数
を示す。Examples include the following: The π substituent constant is shown in parentheses.
−CONH1(−1,49) 、−COtH(−〇、、
32)、−COCHz(0,55) 、−NHCOCH
s(0,97)、−CHzCHtCOzH(−0,29
)、−CHz CHtN H! (−0,08)、=S
CHzCO*H(−0,31)、
−CHtCOtH(−0,72)、
−5CH1CONH1(−0,97)、−S CH*
C−CH5(−0,43)、一3CH,CH,CO,H
(−0,01)、−OH(−0,67)、−CONHO
H(−0,38)、−CH2OH(−1,03)、−C
N (−0,57)、−CH,CN (−0,57)、
−CHtN Ht (−1,04)、−N HCHO(
−0,98)、−NHCONH2(−1,30)、−N
HCH,(−0,47)、−N HS 01CHz
(−1,18>、−N (SOxcHs)z (−1
,51)、−0CONHz(1,05) 、−0CH
3(0,02)、−Q S OICH3(0,88)、
OCOCHs(0,64)、−〇CHICOOH
(−0,87)、
−S O,N Hl(−1,82)、−3O□CH3(
−1,63)、−5OtN(CH3)t(0,78)、
−OCH,CONH2(−1,37) 、−CNHO
H(−1,87)。-CONH1(-1,49), -COtH(-〇,,
32), -COCHz(0,55), -NHCOCH
s(0,97), -CHzCHtCOzH(-0,29
), -CHz CHtNH! (-0,08),=S
CHzCO*H (-0,31), -CHtCOtH (-0,72), -5CH1CONH1 (-0,97), -S CH*
C-CH5(-0,43), -3CH,CH,CO,H
(-0,01), -OH(-0,67), -CONHO
H(-0,38), -CH2OH(-1,03), -C
N (-0,57), -CH,CN (-0,57),
-CHtN Ht (-1,04), -N HCHO(
-0,98), -NHCONH2(-1,30), -N
HCH, (-0,47), -N HS 01CHz
(-1,18>, -N (SOxcHs)z (-1
,51), -0CONHz(1,05), -0CH
3(0,02), -QSOICH3(0,88),
OCOCHs(0,64), -〇CHICOOH
(-0,87), -SO,N Hl(-1,82), -3O□CH3(
-1,63), -5OtN(CH3)t(0,78),
-OCH,CONH2(-1,37), -CNHO
H(-1,87).
一般式(Z−5)においてeは0〜5好ましくは1〜3
の整数を表わす。In general formula (Z-5), e is 0 to 5, preferably 1 to 3
represents an integer.
一般式(Z−1)で表わされる基の例を以下に示す。Examples of the group represented by general formula (Z-1) are shown below.
S CHt CH! CO−H。S CHt CH! CO-H.
S CH! COi H。SCH! COi H.
−5cHzcHcHzOH。-5cHzcHcHzOH.
OH 3CH! CHt N Ht 1 − S CHICHCOtH。OH 3CH! CHt N Ht 1 -S CHICHCOtH.
NH。N.H.
一3CH,CH,NHCH3、
一3CHICHffiNH3ChCH,、−3CH,C
H1NHC○OCH*、
○
一3CH,CH,P (ONa)、、一3CHt
CHz OP (ON a)t、−S CHt C
H! OH。-3CH,CH,NHCH3,-3CHICHffiNH3ChCH,, -3CH,C
H1NHC○OCH*, ○ 13CH,CH,P (ONa), 13CHt
CHz OP (ON a)t, -S CHt C
H! Oh.
−S CHICHlS ozc H3、−3CHtCH
tCH,SO,Na、
−S CHt CH! S 02 N Ht、−S (
CHz)sc OOH。-S CHICHlS ozc H3, -3CHtCH
tCH, SO, Na, -S CHt CH! S 02 N Ht, -S (
Hz)sc OOH.
CH。CH.
一3CHCOOH。13CHCOOH.
CHl 一5CHICHCO○H1 −S CH! CHt S 02 K 。CHl 15CHICHCO○H1 -S CH! CHt S 02 K.
−3CH,CH2CH!OH。-3CH, CH2CH! Oh.
−i式(Z−2)で表わされる基の例を以下に示す。Examples of the group represented by the -i formula (Z-2) are shown below.
S CHz CH! S CHx CHt○H2−3C
H,CH,SCH,C0OH。S CHz CH! S CHx CHt○H2-3C
H, CH, SCH, COOH.
−3CHICM!SCH,CHICOOH。-3CHICM! SCH, CHICOOH.
−3CHzCHzOCHzCHtOH。-3CHzCHzOCHzCHtOH.
−S CH! CHt OCHt CHz OHl−3
CHICH,OCH,CHl0H1−3CH,cHt
CCHt○H1
−S CHt CON HCHt COOH。-SCH! CHt OCHt CHz OHl-3
CHICH,OCH,CH10H1-3CH,cHt
CCHt○H1 -S CHt CON HCHt COOH.
−3(CHICH!0)30H。-3 (CHICH!0) 30H.
−S CHX C)(x N (CHt COOH)
t、−3CHICH,5OICH,C0OH。-S CHX C) (x N (CHt COOH)
t, -3CHICH, 5OICH, COOH.
一般式(Z−3)で表わされる基の例を以下に示す。Examples of the group represented by general formula (Z-3) are shown below.
−N H(CH−CHt S ) s CHz CH2
0Hl−3(CH,CHtS)、CH,CH,○H1−
ocLcozNc++tc+hscHzcozoo 。-NH(CH-CHtS)s CHz CH2
0Hl-3 (CH, CHtS), CH, CH, ○H1-
ocLcozNc++tc+hscHzcozoo.
よ)Iコ
−NH(CHzCH,5)xCHtCHzNHz、S
CH! CHx S CH! CHCHz S CHt
CHff。yo) Iko-NH(CHzCH,5)xCHtCHzNHz,S
CH! CHx S CH! CHCHHz S CHt
CHff.
、りH 一般式(Z−4)で表わされる基の例を以下に示す。,riH Examples of the group represented by general formula (Z-4) are shown below.
一0CHzCHzSSCHxCHt○H1N HCHs
CH! S S CHz CHt N Hz、OCH
t CHz S S CHt CHz C00H。10CHzCHzSSCHxCHt○H1N HCHs
CH! S S CHz CHt N Hz, OCH
t CHz S S CHt CHz C00H.
−3CH,CH25SCHICH,OH。-3CH, CH25SCHICH, OH.
一般式(Z−5)で表わされる基の例を以下に示す。Examples of the group represented by general formula (Z-5) are shown below.
NH2 一般式(Z−5)で表わされる基の中ではり。NH2 Among the groups represented by general formula (Z-5):
が複素環基である基が好ましい。is a heterocyclic group is preferred.
一般式(1)で表わす化合物においてAはカプラー残基
が好ましく、T3、T2及びBは用いない方が好ましく
、Zは一般式(Z−1)、(Z−4)、及び(Z−5)
で表わされる基が好ましく、(Z−1)で表わされる基
がさらに好ましい。In the compound represented by general formula (1), A is preferably a coupler residue, T3, T2 and B are preferably not used, and Z is a coupler residue of general formula (Z-1), (Z-4), and (Z-5). )
A group represented by (Z-1) is preferred, and a group represented by (Z-1) is more preferred.
次に本発明において用いられる漂白促進剤放出型化合物
の具体例を示すが、本発明はこれらに限定されることは
ない。Next, specific examples of the bleach accelerator-releasing compound used in the present invention will be shown, but the present invention is not limited thereto.
(B−リ (B−9 r〜 G−■ ω−η u (B−8) 浦 CB−9) n■ H ω−10) CB−11) 0■ (B−12) I (B−13) 1l (B−15) CB−16) (B−17) CB−18) H3 (B−19) H ω−20) H LatlzuJzrl (B−22) (B−23) (B−24) H しl ω−刃 し1 ω−m CB−28) G3−30) ’LH2lしNzしυ21 ■、五’ C)l。(B-li (B-9 r~ G-■ ω−η u (B-8) Ura CB-9) n■ H ω-10) CB-11) 0■ (B-12) I (B-13) 1l (B-15) CB-16) (B-17) CB-18) H3 (B-19) H ω-20) H LatlzuJzrl (B-22) (B-23) (B-24) H Shil ω-blade 1 ω-m CB-28) G3-30) 'LH2l and Nzshiυ21 ■, 5’ C)l.
(B−41)
(B−0
H
ω−0)
謬
0CONllCH,CI(2父)12CIlδ仰2CH
20H(B−44)
0)l
(B−〇
本発明において用いられる前記漂白促進剤放出型化合物
は例えば特開昭61−201247号、同62−173
467号、同62−24’7363号、特願昭61−2
52847号、同61−268870号、同61−26
8871号、同61−268872号、同62−490
81号、同62−90442号及び同62−18693
9号に記載の方法により合成することができる。(B-41) (B-0 H ω-0) 0CONllCH, CI (2 father) 12CIlδ 2CH
20H(B-44) 0)l (B-0 The bleach accelerator-releasing compound used in the present invention is disclosed in, for example, JP-A-61-201247 and JP-A-62-173.
No. 467, No. 62-24'7363, Patent Application No. 61-2
No. 52847, No. 61-268870, No. 61-26
No. 8871, No. 61-268872, No. 62-490
No. 81, No. 62-90442 and No. 62-18693
It can be synthesized by the method described in No. 9.
本発明に係わる漂白促進剤放出化合物(BAR化合物)
の感光材料への添加量は、感光材料1ボ当りlXl0−
’モル〜lXl0−’モルが好ましく、特にlXl0−
’モル−5X10−”モルが好ましい0本発明に係わる
漂白促進剤放出化合物は、感光材料のすべての層に添加
することができるが、感光性乳剤層に添加することが好
ましく、更にはより多くの感光性乳剤層に添加すると、
効果が著しくなる。Bleach accelerator releasing compound (BAR compound) according to the present invention
The amount of addition to the photosensitive material is lXl0- per 1 photosensitive material.
'molar to lXl0-' molar is preferred, especially lXl0-
The bleach accelerator-releasing compound according to the present invention can be added to all layers of the light-sensitive material, but it is preferably added to the light-sensitive emulsion layer, and even more When added to the photosensitive emulsion layer of
The effect becomes significant.
脱銀不良は感光材料のすべての乳剤層で均一に起ること
もあるが特定の層で起ることが多く、その脱銀不良の発
生している層に添加するとより効果的である。Desilvering defects may occur uniformly in all emulsion layers of a light-sensitive material, but they often occur in a specific layer, and it is more effective to add to the layer where the desilvering defect has occurred.
本発明の化合物をシアン発色層に用いる場合には、5−
アミドナフトール及びウレイドフェノールの構造を有す
る化合物を用いると、酸化力の低下した漂白浴で処理し
た時に生じる濃度低下が少なく有利である。その代表的
な化合物はB−4、B−5、B−6、B−7、B−8、
B−9、B−20、B−17に挙げであるがこれらに限
定されるものではない。When the compound of the present invention is used in a cyan coloring layer, 5-
The use of compounds having the structures of amidonaphthol and ureidophenol is advantageous because the decrease in concentration that occurs when treated in a bleaching bath with reduced oxidizing power is small. The representative compounds are B-4, B-5, B-6, B-7, B-8,
B-9, B-20, and B-17 are listed, but the invention is not limited to these.
本発明の感光材料には公知の写真用添加剤が使用でき、
リサーチ・ディスクロージャーN117643および同
18716
の2つのリサーチ・ディスクロージャーに記載されてお
り、下記の表に関連する記載箇所を示した。Known photographic additives can be used in the light-sensitive material of the present invention.
It is described in two Research Disclosures, Research Disclosure N117643 and Research Disclosure N18716, and the relevant descriptions are shown in the table below.
添加剤種類 RD17643 RD18716
1 化学増感剤 23頁 648頁右欄2恐度上昇剤
同上
4 増 白 剤 24頁8 色素画像安
定剤 25頁
9 硬 膜 剤 26頁 651頁左欄10
バインダー 26頁 同上11 可塑剤、潤滑
剤 27頁 650頁右右下 止 剤
本発明には種々のカラーカプラーを使用することができ
、その具体例は前出のリサーチ・ディスクロージャー(
RD)魚17643、■−〇−Gに記載された特許に記
載されている。Additive type RD17643 RD18716
1 Chemical sensitizers Page 23 Page 648 Right column 2 Intensity increasing agents
Same as above 4 Brightening agent page 24 8 Dye image stabilizer page 25 9 Hardening agent page 26 Page 651 left column 10
Binder, page 26 Same as above 11 Plasticizer, lubricant, page 27, page 650, lower right corner Stopper Various color couplers can be used in the present invention, and specific examples thereof can be found in the aforementioned Research Disclosure (
RD) Fish 17643, described in the patent described in ■-〇-G.
イエローカプラーとしては、例えば米国特許第3.93
3,501号、同第4,022,620号、同第4,3
26,024号、同第4,401゜752号、特公昭5
8−10739号、英国特許第1,425,020号、
同第1. 476、 760号、等に記載のものが好ま
しい。As a yellow coupler, for example, U.S. Patent No. 3.93
No. 3,501, No. 4,022,620, No. 4,3
No. 26,024, No. 4,401゜752, Special Publication No. 5
No. 8-10739, British Patent No. 1,425,020,
Same 1st. 476, 760, etc. are preferred.
マゼンタカプラーとしては5−ピラゾロン系及びピラゾ
ロアゾール系の化合物が好ま°シ<、米国特許第4.3
10,619号、同第4.351゜897号、欧州特許
第73,636号、米国特許第3,061,432号、
同第3. 725’、 067号、リサーチ・ディス
クロージ; −魚242’10(1984年6月)、特
開昭60−33552号、リサーチ・ディスクロージャ
ーNth 24230(19a4年6月)、特開昭60
−43659号、米国特許第4,500,630号、同
第4.540・ 654号等に記載のものが特に好まし
し)。As magenta couplers, 5-pyrazolone and pyrazoloazole compounds are preferred, US Pat. No. 4.3.
10,619, 4.351°897, European Patent No. 73,636, U.S. Patent No. 3,061,432,
Same 3rd. 725', No. 067, Research Disclosure; -Uo 242'10 (June 1984), JP-A-60-33552, Research Disclosure Nth 24230 (June 19a4), JP-A-60
Particularly preferred are those described in US Pat. No. 4,500,630, US Pat. No. 4,540,654, etc.).
シアンカプラーとしては、フェノール系及びナフトール
系カプラーが挙げられ、米国特許第4゜052.212
号、同第4,146.396号、同第4,228,23
3号、同第4. 296.200号、同第2,369.
929号、同第2,801.171号、同第2,772
.162号、同第2,895.826号、同第3. 7
72. 002号、同第3,158,308号、同第4
,334.011号、同第4.327,173号、***
特許公開第3,329.729号、欧州特許第121.
365A号、米国特許第3,446,622号、同第4
.333,999号、同第4,451.559号、同第
4,427,767号、欧州特許第161.626A号
等に記載のものが好ましい。Cyan couplers include phenolic and naphthol couplers, and are described in U.S. Pat. No. 4,052,212.
No. 4,146.396, No. 4,228,23
No. 3, No. 4. No. 296.200, No. 2,369.
No. 929, No. 2,801.171, No. 2,772
.. No. 162, No. 2,895.826, No. 3. 7
72. No. 002, No. 3,158,308, No. 4
, No. 334.011, No. 4.327,173, West German Patent Publication No. 3,329.729, European Patent No. 121.
No. 365A, U.S. Patent No. 3,446,622, U.S. Patent No. 4
.. Preferred are those described in No. 333,999, No. 4,451.559, No. 4,427,767, European Patent No. 161.626A, and the like.
発色色素の不要吸収を補正するためのカラード・カプラ
ーは、リサーチ・ディスクロージャー隘17643の■
−G項、米国特許第4,163゜670号、特公昭57
−39413号、米国特許第4,004,929号、同
第4. 138. 258号、英国特許第1,146.
368号に記載のものが好ましい。Colored couplers for correcting unnecessary absorption of coloring dyes are described in Research Disclosure No. 17643.
- Section G, U.S. Patent No. 4,163゜670, Japanese Patent Publication No. 1983
-39413, U.S. Patent No. 4,004,929, U.S. Patent No. 4. 138. No. 258, British Patent No. 1,146.
The one described in No. 368 is preferred.
発色色素が適度な拡散性を有するカプラーとしては、米
国特許第4,366.237号、英国特許第2,125
.570号、欧州特許第96,570号、***特許(公
開)第3,234,533号に記載のものが好ましい。Couplers whose coloring dyes have appropriate diffusivity include U.S. Patent No. 4,366.237 and British Patent No. 2,125.
.. 570, European Patent No. 96,570 and German Patent Publication No. 3,234,533 are preferred.
ポリマー化された色素形成カプラーの典型例は、米国特
許第3,451,820号、同第4.080.211号
、同第4,367.282号、英国特許第2,102.
173号等に記載されている。Typical examples of polymerized dye-forming couplers are U.S. Pat. No. 3,451,820, U.S. Pat. No. 4.080.211, U.S. Pat.
It is described in No. 173, etc.
カップリングに伴って写真的に有用な残基を放出するカ
プラーもまた本発明で好ましく使用できる。現像押割剤
を放出するDIRカプラーは、前述のRD17643、
■〜F項に記載された特許、特開昭57−151944
号、同57−154234号、同60−184248号
、米国特許第4゜248.962号に記載されたものが
好ましい。Couplers that release photographically useful residues upon coupling are also preferably used in the present invention. The DIR coupler that releases the developer pushing agent is the above-mentioned RD17643,
Patents listed in Sections ■-F, Japanese Patent Application Laid-Open No. 57-151944
Preferred are those described in No. 57-154234, No. 60-184248, and U.S. Pat.
現像時に画像状に造核剤もしくは現像促進剤を放出する
カプラーとしては、英国特許第2.097.140号、
同第2,131,188号、特開昭59−157638
号、同59−170840号に記載のものが好ましい。As a coupler that releases a nucleating agent or a development accelerator imagewise during development, British Patent No. 2.097.140;
No. 2,131,188, JP 59-157638
No. 59-170840 is preferred.
その他、本発明の感光材料に用いることのできるカプラ
ーとしては、米国特許第4.130.427号等に記載
の競争カプラー、米国特許第4゜283.472号、同
第4,338,393号、同第4,310.618号等
に記載の多光量カプラー、特開昭60−185950、
特開昭62−24252等に記載のDIRレドックス化
合物もしくはDIRカプラー放出カプラー又はDIRカ
プラー放出カプラーもしくはレドックス、欧州特許第1
73,302A号に記載の離脱後後色する色素を放出す
るカプラー、
米国特許第4.5
53.477号等に記載のリガンド放出カプラー等が挙
げられる。In addition, examples of couplers that can be used in the photosensitive material of the present invention include competitive couplers described in U.S. Pat. No. 4,130,427, U.S. Pat. , the multi-light coupler described in JP-A-60-185950, etc.
DIR redox compound or DIR coupler releasing coupler or DIR coupler releasing coupler or redox described in JP-A-62-24252 etc., European Patent No. 1
Examples thereof include couplers that release dyes that undergo discoloration after separation, as described in No. 73,302A, and ligand-releasing couplers as described in U.S. Pat.
本発明に於いては、マゼンタカプラーとしては、色相の
点からピラゾロアゾール型のマゼンタカプラーが好まし
い、特に青光吸収帯の副吸収が少ないため、カラードカ
プラーを減少させることができ、本発明の高感度感光材
料では特に有利である。In the present invention, as the magenta coupler, a pyrazoloazole type magenta coupler is preferable from the viewpoint of hue.In particular, since the side absorption in the blue light absorption band is small, colored couplers can be reduced. This is particularly advantageous for highly sensitive photosensitive materials.
ピラゾロアゾール型のカプラーは、マゼンタ色素形成成
分の全量であってもよいし、他の5−ピラゾロン型のカ
プラーと併用して用いてもよい。The pyrazoloazole type coupler may be the entire magenta dye-forming component or may be used in combination with other 5-pyrazolone type couplers.
次に特に好ましいマゼンタカプラーの例を示す。Next, examples of particularly preferred magenta couplers will be shown.
(M−1)
(M−2)
(M−3)
しn3
(M−4)
(M−5)
(M−6)
n−Ca !Lx
(M−7)
(M−8>
(M−9)
リ しS 1111LLノ(M−1o)
(M−11)
(M−12)
CM−13)
(M−14)
(M−15)
(M−16)
(M−18)
(M−19)
(M−20>
CnHg+
(M−22)
(M−23)
(M−24)
(M−25)
+CH1−CH旨 千CHI −CH旨(M−2
6)
Hi
□
−(−CH2−C汁マ ÷CHt−CH
汁7X#−40/60 (重l)
(M−27)
千CH,−CH旨 +cH,−CH旨x/y=5
0150 (重り
(M−28)
Hi
+CL−CH汁マ +CH,−CHl−7
x/y−55/45 (重量)
(M−29)
本発明に使用するカプラーは、種々の公知分散方法によ
り恐光材料に4人できる。(M-1) (M-2) (M-3) n3 (M-4) (M-5) (M-6) n-Ca! Lx (M-7) (M-8> (M-9) Li S 1111LLノ (M-1o) (M-11) (M-12) CM-13) (M-14) (M-15) (M-16) (M-18) (M-19) (M-20> CnHg+ (M-22) (M-23) (M-24) (M-25) +CH1-CH 1,000CHI -CH (M-2
6) Hi □ -(-CH2-C juice ma ÷CHt-CH
Soup 7
0150 (Weight (M-28) Hi +CL-CH Soup +CH, -CHl-7
x/y-55/45 (weight) (M-29) The coupler used in the present invention can be made into a photophobic material by various known dispersion methods.
水中油滴分散法に用いられる高沸点溶媒の例は米国特許
第2,322,027号などに記載されている。Examples of high boiling point solvents used in the oil-in-water dispersion method are described in US Pat. No. 2,322,027 and the like.
水中油滴分散法に用いられる常圧での沸点が175℃以
上の高沸点有機溶剤の具体例としては、フタル酸エステ
ル類(ジブチルフタレート、ジシクロへキシルフタレー
ト、ジー2−エチルへキシルフタレート、デシルフタレ
ート、ビス(2,4−ジ−t−アミルフェニル)フタレ
ート、ビス(2,4−ジ−t−アミルフェニル)イソフ
タレート、ビス(1,1−ジエチルプロピル)フタレー
トなど)、リン酸またはホスホン酸のエステル類(トリ
フエルホスフェート、トリクレジルホスフェート、2−
エチルへキシルジフェニルホスフェート、トリシクロヘ
キシルホスフェート、トリー2−エチルへキシルホスフ
ェート、トリドデシルホスフェート、トリブトキシエチ
ルホスフェート、トリクロロプロピルホスフェート、ジ
−2−エチルへキシルフェニルホスホ?−トなど)、安
息香酸エステル類(2−エチルへキシルベンゾエート、
ドデシルベンゾエート、2−エチルへキシル−p−ヒド
ロキシベンゾエートなど)、アミド:W(N、N−ジエ
チルドデカンアミド、N、N−ジエチルラウリルアミド
、N−テトラデシルピロリドンなど)、アルコール類ま
たはフェノール類(インステアリルアルコール、2.4
−ジーter t−アミルフェノールなど)、脂肪族カ
ルボン酸エステル類(ヒス(2−エチルヘキシル)セバ
ケート、ジオクチルアゼレート、グリセロールトリブチ
レート、インステアリルラクテート、トリオクチルシト
レートなど)、アニリン誘導体(N、 N−ジブチル
−2−ブトキシ−5−tart−オクチルアニリンなど
)、炭化水素類(パラフィン、ドデシルベンゼン、ジイ
ソプロピルナフタレンなど)などが挙げられる。また補
助溶剤としては、沸点が約30℃以上、好ましくは50
℃以上約160℃以下の有機溶剤などが使用でき、典型
例としては酢酸エチル、酢酸ブチル、プロピオン酸エチ
ル、メチルエチルケトン、シクロヘキサノン、2−エト
キシエチルアセテート、ジメチルホルムアミドなどが挙
げられる。Specific examples of high-boiling organic solvents with a boiling point of 175°C or higher at normal pressure used in the oil-in-water dispersion method include phthalic acid esters (dibutyl phthalate, dicyclohexyl phthalate, di-2-ethylhexyl phthalate, decyl phthalate, bis(2,4-di-t-amylphenyl) phthalate, bis(2,4-di-t-amylphenyl) isophthalate, bis(1,1-diethylpropyl) phthalate, etc.), phosphoric acid or phosphonic acid Acid esters (trifel phosphate, tricresyl phosphate, 2-
Ethylhexyl diphenyl phosphate, tricyclohexyl phosphate, tri-2-ethylhexyl phosphate, tridodecyl phosphate, tributoxyethyl phosphate, trichloropropyl phosphate, di-2-ethylhexyl phenyl phosphate? ), benzoic acid esters (2-ethylhexylbenzoate, etc.), benzoic acid esters (2-ethylhexylbenzoate,
dodecyl benzoate, 2-ethylhexyl-p-hydroxybenzoate, etc.), amides: W (N,N-diethyldodecanamide, N,N-diethyl laurylamide, N-tetradecylpyrrolidone, etc.), alcohols or phenols ( Instearyl alcohol, 2.4
-diter t-amylphenol, etc.), aliphatic carboxylic acid esters (his(2-ethylhexyl) sebacate, dioctyl azelate, glycerol tributyrate, instearyl lactate, trioctyl citrate, etc.), aniline derivatives (N, N-dibutyl-2-butoxy-5-tart-octylaniline, etc.), hydrocarbons (paraffin, dodecylbenzene, diisopropylnaphthalene, etc.), and the like. In addition, as an auxiliary solvent, the boiling point is about 30°C or higher, preferably 50°C or higher.
An organic solvent having a temperature of 160°C or higher can be used, and typical examples thereof include ethyl acetate, butyl acetate, ethyl propionate, methyl ethyl ketone, cyclohexanone, 2-ethoxyethyl acetate, dimethylformamide, and the like.
ラテックス分散法の工程、効果および含浸用のラテック
スの具体例は、米国特許第4,199゜363号、***
特許出願(OLS)第2.541゜274号および同第
2,541,230号などに記載されている。Specific examples of latex dispersion processes, effects, and latex for impregnation include U.S. Pat. It is described in.
本発明は種々のカラー感光材料に適用することができる
。一般用もしくは映画用のカラーネガフィルム、スライ
ド用もしくはテレビ用のカラー反転フィルム、カラーペ
ーパー、カラーポジフィルムおよびカラー反転ペーパー
などを代表例として挙げることができる。The present invention can be applied to various color photosensitive materials. Typical examples include color negative film for general use or movies, color reversal film for slides or television, color paper, color positive film, and color reversal paper.
本発明に使用できる適当な支持体は、例えば、前述のR
D、寛17643の28頁、および回置18716の6
47頁右欄から648頁左欄に記載されている。Suitable supports that can be used in the present invention include, for example, the above-mentioned R
D, Kan 17643, page 28, and rotation 18716, 6
It is described from the right column on page 47 to the left column on page 648.
本発明に従ったカラー写真窓光材料は、前述のRD、隘
17643の28〜29頁、および同徹18716の6
51左欄〜右欄に記載された通常の方法によって現像処
理することができろ。The color photographic window light material according to the present invention is described in the aforementioned RD, No. 17643, pages 28-29, and Dotetsu No. 18716, No. 6.
51 Can be developed by the usual methods described in the left column to right column.
本発明の感光材料の現像処理に用いる発色現像液は、好
ましくは芳香族第一級アミン系発色現像主薬を主成分と
するアルカリ性水溶液である。この発色現像主薬として
は、アミノフェノール系化合物も育用であるが、p−フ
ェニレンジアミン系化合物が好ましく使用され、その代
表例としては3−メチル−4−アミノ−N、N−ジエチ
ルアニリン、3−メチル−4−アミノ−N−エチル−N
−β−ヒドロキシエチルアニリン、3−メチル−4−ア
ミノ−N−エチル−N−β−メタンスルホンアミドエチ
ルアニリン、3−メチル−4−アミノ−N−エチル−N
−β−メトキシエチルアニリン及びこれらのg酸塩、塩
酸塩もしくはp−トルエンスルホン酸塩などが挙げられ
る。これらの化合物は目的に応じ2種以上併用すること
もできる。The color developing solution used in the development of the light-sensitive material of the present invention is preferably an alkaline aqueous solution containing an aromatic primary amine color developing agent as a main component. Although aminophenol compounds are also used as color developing agents, p-phenylenediamine compounds are preferably used. Representative examples include 3-methyl-4-amino-N, N-diethylaniline, -methyl-4-amino-N-ethyl-N
-β-hydroxyethylaniline, 3-methyl-4-amino-N-ethyl-N-β-methanesulfonamidoethylaniline, 3-methyl-4-amino-N-ethyl-N
-β-methoxyethylaniline and their g-acid salts, hydrochlorides, p-toluenesulfonates, and the like. Two or more of these compounds can be used in combination depending on the purpose.
発色現像液は、アルカリ金属の炭酸塩、ホウ酸塩もしく
はリン酸塩のようなpHff1衝剤、臭化物塩、沃化物
塩、ベンズイミダゾール類、ヘンジチアゾール類もしく
はメルカプト化合物のような現像抑制剤またはカブリ防
止剤などを含むのが一般的である。また必要に応じて、
ヒドロキシルアミン、ジエチルヒドロキシルアミン、亜
硫酸塩ヒドラジン類、フェニルセミカルバジド類、トリ
エタ、/−ルアミン、カテコールスルホン酸類、トリエ
チレンジアミン(1,4−ジアザビシクロ(2゜2.2
〕オクタン)類の如き各種保恒剤、エチレングリコール
、ジエチレングリコールのような育機溶剤、ベンジルア
ルコール、ポリエチレングリコール、四級アンモニウム
塩、アミン類のような現像促進剤、色素形成カプラー、
競争カプラー、ナトリウムボロンハイドライドのような
カブラセ剤、1−フェニル−3−ピラゾリドンのような
補助現像主薬、粘性付与剤、アミノポリカルボン酸、ア
ミノポリホスホン酸、アルキルホスホン酸、ホスホノカ
ルボン酸に代表されるような各種キレート剤、例えば、
エチレンジアミン四酢酸、ニトリロ三酢酸、ジエチレン
トリアミン五酢酸、シクロヘキサンジアミン四酢酸、ヒ
ドロキシエチルイミノジ酢酸、1−ヒドロキシエチリデ
ン−1,1−ジホスホン酸、ニトリロ−N、N、N−)
リメチレンホスホン酸、エチレンジアミン−N、N。The color developer may contain pHff1 buffers such as alkali metal carbonates, borates or phosphates, development inhibitors such as bromide salts, iodide salts, benzimidazoles, hendithiazoles or mercapto compounds, or fogging agents. It generally contains an inhibitor. Also, if necessary,
Hydroxylamine, diethylhydroxylamine, sulfite hydrazines, phenylsemicarbazides, triethylamine, catecholsulfonic acids, triethylenediamine (1,4-diazabicyclo(2゜2.2
] Various preservatives such as octane), growth solvents such as ethylene glycol and diethylene glycol, development accelerators such as benzyl alcohol, polyethylene glycol, quaternary ammonium salts, and amines, dye-forming couplers,
Competitive couplers, fogging agents such as sodium boron hydride, auxiliary developing agents such as 1-phenyl-3-pyrazolidone, tackifiers, aminopolycarboxylic acids, aminopolyphosphonic acids, alkylphosphonic acids, phosphonocarboxylic acids. Various chelating agents such as
Ethylenediaminetetraacetic acid, nitrilotriacetic acid, diethylenetriaminepentaacetic acid, cyclohexanediaminetetraacetic acid, hydroxyethyliminodiacetic acid, 1-hydroxyethylidene-1,1-diphosphonic acid, nitrilo-N,N,N-)
Rimethylenephosphonic acid, ethylenediamine-N,N.
N’、N’−テトラメチレンホスホン酸、エチレングリ
コ−ル(0−ヒドロキシフェニル酢酸)及びそれらの塩
を代表例として上げることができる。Representative examples include N',N'-tetramethylenephosphonic acid, ethylene glycol (0-hydroxyphenylacetic acid), and salts thereof.
また反転処理を実施する場合は通常黒白現像を行ってか
ら発色現像する。この黒白現像液には、ハイドロキノン
などのジヒドロキシベンゼン類、1−フェニル−3−ピ
ラゾリドンなどの3−ピラゾリドン類またはN−メチル
−p−アミノフェノールなどのアミノフェノール類など
公知の黒白現像主薬を単独であるいは組み合わせて用い
ることができる。Further, when performing reversal processing, black and white development is usually performed and then color development is performed. This black and white developer contains known black and white developing agents such as dihydroxybenzenes such as hydroquinone, 3-pyrazolidones such as 1-phenyl-3-pyrazolidone, or aminophenols such as N-methyl-p-aminophenol. Alternatively, they can be used in combination.
これらの発色現a液及び黒白現像液のpH9〜12であ
ることが一般的である。またこれらの現像液の補充量は
、処理するカラー写真怒光材料にもよるが、一般に5光
材料1平方メートル当たり31以下であり、補′充液中
の臭化物イオン濃度を低減させておくことにより500
m1t以下にすることもできる。補充量を低減する場合
には処理槽の空気との接触面積を小さくすることによっ
て液の蒸発、空気酸化を防止することが好ましい。また
現像液中の臭化物イオンの蓄積を抑える手段を用いるこ
とにより補充量を低減することもできる。The pH of these color developing solutions and black and white developing solutions is generally 9 to 12. The amount of replenishment of these developing solutions depends on the color photographic material to be processed, but is generally less than 31 per square meter of 5-light material, and by reducing the bromide ion concentration in the replenishing solution. 500
It can also be made less than m1t. When reducing the amount of replenishment, it is preferable to prevent evaporation of the liquid and air oxidation by reducing the area of contact with the air in the processing tank. Furthermore, the amount of replenishment can be reduced by using means for suppressing the accumulation of bromide ions in the developer.
発色現像処理の時間は通常2〜5分の間で設定されるが
高温、高p Hとし、且つ発色現像主薬を高濃度に使用
することにより、更に処理時間の短縮を図ることもでき
る。The time for color development processing is usually set between 2 and 5 minutes, but the processing time can be further shortened by using high temperature, high pH, and high concentration of color developing agent.
発色現像後の写真乳剤層は通常漂白処理される。After color development, the photographic emulsion layer is usually bleached.
漂白処理は定着処理と同時に行なわれてもよいしく漂白
定着処理)、個別に行なわれてもよい。更に処理の迅速
化を図るため、漂白処理後漂白定着処理する処理方法で
もよい。さらに二種の連続した漂白定着浴で処理するこ
と、漂白定着処理の前に定着処理すること、又は漂白定
着処理後漂白処理することも目的に応じ任意に実施でき
る。漂白剤としては、例えば鉄(■)、コバル) (I
II)、クロム(■)、銅(II)などの多価金属の化
合物、過酸類、キノン類、ニトロ化合物等が用いられる
。The bleaching process may be carried out simultaneously with the fixing process (bleach-fixing process) or separately. Furthermore, in order to speed up the processing, a processing method may be used in which bleaching is followed by bleach-fixing. Furthermore, treatment with two consecutive bleach-fixing baths, fixing treatment before bleach-fixing treatment, or bleaching treatment after bleach-fixing treatment can be carried out as desired depending on the purpose. Examples of bleaching agents include iron (■), Kobal) (I
Compounds of polyvalent metals such as II), chromium (■), and copper (II), peracids, quinones, nitro compounds, and the like are used.
代表的漂白剤としてはフェリシアン化物;重クロム酸塩
;鉄(■)、もしくはコバルト([11)の有機錯塩、
例えばエチレンジアミン四酢酸、ジエチレ
/
ントリアミン五酢酸、シクロヘキサンジアミン四酢酸、
メチルイミノニ酢酸、1.3−ジアミノプロパン四酢酸
、グリコールエーテルジアミン四酢酸、などのアミノポ
リカルボン酸類もしくはクエン酸、酒石酸、リンゴ酸な
どの錯塩;過硫酸塩;臭素酸塩;過マンガン酸塩;ニト
ロベンゼン類などを用いることができる。これらのうち
エチレンジアミン四酢酸鉄(m)錯塩を始めとするアミ
ノポリカルボン酸鉄(I[[)錯塩及び過硫酸塩は迅速
処理と環境汚染防止の観点から好ましい、さらにアミノ
ポリカルボン酸鉄(Ill)錯塩は漂白液においても、
漂白定着液においても特に有用である。Typical bleaching agents include ferricyanide; dichromate; organic complex salts of iron (■) or cobalt ([11)];
For example, ethylenediaminetetraacetic acid, diethyl/triaminepentaacetic acid, cyclohexanediaminetetraacetic acid,
Aminopolycarboxylic acids such as methyliminodiacetic acid, 1,3-diaminopropanetetraacetic acid, glycol ether diamine tetraacetic acid, or complex salts of citric acid, tartaric acid, malic acid, etc.; persulfates; bromates; permanganates; nitrobenzene etc. can be used. Among these, aminopolycarboxylic acid iron (I [[) complex salts and persulfates, including ethylenediaminetetraacetic acid iron (m) complex salts, are preferable from the viewpoint of rapid processing and environmental pollution prevention. ) Complex salts are also present in bleaching solutions.
It is also particularly useful in bleach-fix solutions.
これらのアミノポリカルボン酸鉄(I[I)錯塩を用い
た漂白液又は漂白定着液のpHは通常5.5〜8である
が、処理の迅速化のために、さらに低いpHで処理する
こともできる。The pH of the bleaching solution or bleach-fixing solution using these aminopolycarboxylic acid iron(I[I) complex salts is usually 5.5 to 8, but in order to speed up the processing, the pH may be lowered. You can also do it.
漂白液、漂白定着液及びそれらの前浴には、必要に応じ
て漂白促進剤を使用することができる。A bleach accelerator may be used in the bleaching solution, bleach-fixing solution, and their prebaths, if necessary.
有用な漂白促進剤の具体例は、次の明細書に記載されて
いる:米国特許第3,893,858号、***特許第1
,290,812号、同2,059゜988号、特開昭
53−32,736号、同53−57.831号、同5
3−37.418号、同53−72.623号、同53
−95.630号、同53−95,631号、同53−
10.4232号、同53−124,424号、同53
−141.623号、同53−28.426号、リサー
チ・ディスクロージャー魚17,129号(1978年
7月)などに記載のメルカプト基またはジスルフィド基
を有する化合物;特開昭50−140.129号に記載
のチアゾリジン誘導体;特公昭45−8,506号、特
開昭52−20.832号、同53−32,735号、
米国特許第3゜706.561号に記載のチオ尿素誘導
体;***特許第1,127,715号、特開昭58−1
6゜235号に記載の沃化物塩;***特許第966゜4
10号、同2,748,430号に記載のポリオキシエ
チレン化合物類;特公昭45−8836号記載のポリア
ミン化合物;その他特開昭49−42.434号、同4
9−59.644号、同53−94.927号、同54
−35,727号、同55−26,506号同58−1
63,940号記載の化合物;臭化物イオン等が使用で
きる。Specific examples of useful bleach accelerators are described in U.S. Pat. No. 3,893,858, German Pat.
, No. 290,812, No. 2,059°988, JP-A-53-32,736, No. 53-57.831, No. 5
No. 3-37.418, No. 53-72.623, No. 53
-95.630, 53-95,631, 53-
No. 10.4232, No. 53-124,424, No. 53
-141.623, 53-28.426, Research Disclosure Fish No. 17,129 (July 1978), etc. Compounds having a mercapto group or disulfide group; JP-A-50-140.129 Thiazolidine derivatives described in JP-B No. 45-8,506, JP-A No. 52-20.832, JP-A No. 53-32,735,
Thiourea derivatives described in U.S. Pat. No. 3.706.561; West German Pat.
6゜235; West German Patent No. 966゜4
10, polyoxyethylene compounds described in JP-A No. 2,748,430; polyamine compounds described in JP-A No. 45-8836; and other JP-A-49-42.434, JP-A-4
No. 9-59.644, No. 53-94.927, No. 54
-35,727, 55-26,506, 58-1
Compounds described in No. 63,940; bromide ions, etc. can be used.
なかでもメルカプト基またはジスルフィド基を存する化
合物が促進効果が大きい観点で好ましく、特に米国枠
許第3,893,858号、西特許第1,290,81
2号、特開昭53−95,630号に記載の化合物が好
ましい、更に、米国特許第4.552,834号に記載
の化合物も好ましい、これらの漂白促進剤は感材中に添
加してもよい、撮影用のカラー感光材料を漂白定着する
ときにこれらの漂白促進剤は特に有効である。Among these, compounds having a mercapto group or a disulfide group are preferable from the viewpoint of having a large promoting effect, and are particularly suitable for the US framework.
Patent No. 3,893,858, West Patent No. 1,290,81
No. 2, JP-A No. 53-95,630 is preferred, and compounds described in U.S. Pat. No. 4,552,834 are also preferred. These bleach accelerators can be added to the sensitive material. These bleach accelerators are particularly effective when bleach-fixing color light-sensitive materials for photography.
定着剤としてはチオ硫酸塩、チオシアン酸塩、チオエー
テル系化合物、チオ尿素類、多量の沃化物塩等をあげる
ことができるが、チオ硫酸塩の使用が一般的であり、特
にチオ硫酸アンモニウムが最も広範に使用できる。漂白
定着液の保恒剤としては、亜硫酸塩や重亜硫酸塩あるい
はカルボニル重亜硫酸付加物が好ましい。Examples of fixing agents include thiosulfates, thiocyanates, thioether compounds, thioureas, and large amounts of iodide salts, but thiosulfates are commonly used, with ammonium thiosulfate being the most widely used. Can be used for As the preservative for the bleach-fix solution, sulfites, bisulfites, or carbonyl bisulfite adducts are preferred.
本発明のハロゲン化銀カラー写真感光材料は、脱銀処理
後、水洗及び/又は安定工程を経るのが一般的である。The silver halide color photographic light-sensitive material of the present invention is generally subjected to water washing and/or stabilization steps after desilvering treatment.
水洗工程での水洗水量は、感光材料の特性(例えばカプ
ラー等使用素材による)、用途、更には水洗水温、水洗
タンクの数(段数)、向流、順流等の補充方式、その他
種々の条件によって広範囲に設定し得る。このうち、多
段向流方式における水洗タンク数と水量の関係は、Jo
urnalof the 5ociety of
Motion Picture and T
elevisionEngineers第64e、P、
24B−253(1955年5月号)に記載の方法で、
求めることができる。The amount of water used in the washing process depends on the characteristics of the photosensitive material (for example, depending on the materials used such as couplers), the application, the temperature of the washing water, the number of washing tanks (number of stages), the replenishment method such as countercurrent or forward flow, and various other conditions. Can be set over a wide range. Among these, the relationship between the number of washing tanks and the amount of water in the multistage countercurrent method is
urnalof the 5ociety of
Motion Picture and T
elevision Engineers No. 64e, P.
24B-253 (May 1955 issue),
You can ask for it.
前記文献に記載の多段向流方式によれば、水洗水量を大
幅に減少し得るが、タンク内における水の滞留時間の増
加により、バクテリアが繁殖し、生成した浮遊物が感光
材料に付着する等の問題が生じる0本発明のカラー感光
材料の処理において、このような問題の解決策として、
特願昭61−131.632号に記載のカルシウムイオ
ン、マグネシウムイオンを低減させる方法を極めて有効
に用いることができる。また、特開昭57−8.542
号に記載のイソチアゾロン化合物やサイアベンダゾール
類、塩素化イソシアヌール酸ナトリウム等の塩素系殺菌
剤、その他ベンゾトリアゾール等、堀口博著「防菌防黴
剤の化学」、衛生技術会′dA「微生物の滅菌、殺菌、
防黴技術」、日本防菌防黴学会績「防菌防黴剤事典」に
記載の殺菌剤を用いることもできる。According to the multi-stage countercurrent method described in the above-mentioned literature, the amount of water used for washing can be significantly reduced, but due to the increase in the residence time of water in the tank, bacteria will breed, and the generated suspended matter will adhere to the photosensitive material. In the processing of the color photosensitive material of the present invention, as a solution to such problems,
The method for reducing calcium ions and magnesium ions described in Japanese Patent Application No. 61-131.632 can be used very effectively. Also, JP-A-57-8.542
Chlorinated disinfectants such as isothiazolone compounds, cyabendazole, chlorinated sodium isocyanurate, and other benzotriazoles described in the issue, Hiroshi Horiguchi, "Chemistry of antibacterial and fungicidal agents," Sanitation Technology Association'dA, "Microorganisms. sterilization, sterilization,
It is also possible to use fungicides described in "Anti-fungal Technology" and "Encyclopedia of Antibacterial and Antifungal Agents" published by the Japan Antibacterial and Antifungal Society.
本発明の感光材料の処理における水洗水のpHは、4−
9であり、好ましくは5−8である。水洗水温、水洗時
間も、感光材料の特性、用途等で種々設定し得るが、一
般には、15−45℃で20秒−10分、好ましくは2
5−40℃で30秒−5分の範囲が選択される。更に、
本発明の感光材料は、上記水洗に代り、直接安定液によ
って処理することもできる。このような安定化処理にお
いては、特開昭57−8.543号、同58−14.8
34号、同60−220,345号に記載の公知の方法
はすべて用いることができる。The pH of the washing water in the processing of the photosensitive material of the present invention is 4-
9, preferably 5-8. The washing water temperature and washing time can also be set variously depending on the characteristics of the photosensitive material, its use, etc., but generally it is 20 seconds to 10 minutes at 15-45°C, preferably 20 minutes.
A range of 30 seconds to 5 minutes at 5-40°C is selected. Furthermore,
The light-sensitive material of the present invention can also be directly processed with a stabilizing solution instead of washing with water. In such stabilization treatment, Japanese Patent Application Laid-Open Nos. 57-8.543 and 58-14.8
All known methods described in No. 34 and No. 60-220,345 can be used.
又、前記水洗処理に続いて、更に安定化処理する場合も
あり、その例として、撮影用カラー感光材料の最終浴と
して使用される、ホルマリンと界面活性剤を含有する安
定浴を挙げることができる。Further, following the water washing treatment, a further stabilization treatment may be carried out, such as a stabilizing bath containing formalin and a surfactant, which is used as a final bath for color photosensitive materials for photography. .
この安定浴にも各穏キレート剤や防黴剤を加えることも
できる。A mild chelating agent or a fungicide can also be added to this stabilizing bath.
上記水洗及び/又は安定液の補充に伴うオーバーフロー
液は脱銀工程等信の工程において再利用することもでき
る。The overflow liquid from water washing and/or replenishment of the stabilizing liquid can be reused in other processes such as the desilvering process.
本発明のハロゲン化銀カラー感光材料には処理の簡略化
及び迅速化の目的で発色現像主薬を内蔵しても良い、内
蔵するためには、発色現像主薬の各種プレカーサーを用
いるのが好ましい0例えば米国特許第3.342,59
7号記載のインドアニリン系化合物、同第3,342,
599号、リサーチ・ディスクロージャー14.850
号及び同15.159号記載のシッフ塩基型化合物、同
13.924号記載のアルドール化合物、米国特許第3
.719,492号記載の金属塩錯体、特開昭53−1
35.628号記載のウレタン系化合物を挙げることが
できる。The silver halide color light-sensitive material of the present invention may contain a color developing agent for the purpose of simplifying and speeding up processing. In order to incorporate a color developing agent, it is preferable to use various precursors of the color developing agent. U.S. Patent No. 3.342,59
Indoaniline compound described in No. 7, No. 3,342,
No. 599, Research Disclosure 14.850
Schiff base-type compounds described in No. 15.159 and aldol compounds described in No. 13.924, U.S. Patent No. 3
.. Metal salt complex described in No. 719,492, JP-A-53-1
Examples include urethane compounds described in No. 35.628.
本発明のハロゲン化銀カラー感光材料は、必要に応じて
、発色現像を促進する目的で、各種の1−フェニル−3
−ビラプリトン類を内蔵しても良い、典型的な化合物は
特開昭56−64,339号、同57−144,547
号、および同58−115.438号等記載されている
。The silver halide color light-sensitive material of the present invention may optionally contain various 1-phenyl-3
- Typical compounds that may contain birapritons are JP-A-56-64,339 and JP-A-57-144,547.
No. 58-115.438, etc.
本発明における各種処理液は10℃〜50℃において使
用される。a常は33℃〜38℃の温度が標準的である
が、より高温にして処理を促進し処理時間を短縮したり
、逆により低温にして画質の向上や処理液の安定性の改
良を達成することができる。また、感光材料の路銀のた
め***特許第2.226,770号または米国特許第3
,674.499号に記載のコバルト補力もしくは過酸
化水素補力を用いた処理を行ってもよい。Various treatment liquids in the present invention are used at 10°C to 50°C. The standard temperature is usually 33°C to 38°C, but higher temperatures can be used to accelerate processing and shorten processing time, or lower temperatures can be used to improve image quality and stability of the processing solution. can do. In addition, for the roadside of photosensitive materials, West German Patent No. 2.226,770 or U.S. Patent No. 3
, 674.499 may be carried out using cobalt intensification or hydrogen peroxide intensification.
また、本発明のハロゲン化銀窓光材料は米国特許第4,
500,626号、特開昭60−133449号、同5
9−218443号、同61−238056号、欧州特
許210,660A2号などに記載されている熱現像感
光材料にも適用でき〔実施例〕
以下1本発明を実施例によって具体的に説明する。Further, the silver halide window optical material of the present invention is disclosed in U.S. Patent No. 4,
No. 500,626, JP-A-60-133449, No. 5
The present invention can also be applied to the heat-developable photosensitive materials described in European Patent No. 9-218443, European Patent No. 61-238056, European Patent No. 210,660A2, etc. [Examples] The present invention will be specifically explained below with reference to Examples.
実施例1
下塗りを施した三酢酸セルロースフィルム支持体上に、
下記に示すような組成の各層よりなる多層カラー感光材
料である試料101Σj ’f−’A LT=。Example 1 On a subbed cellulose triacetate film support,
Sample 101Σj 'f-'A LT= is a multilayer color photosensitive material consisting of each layer having the composition shown below.
(感光層の組成)
第1層(ハレーション防止層)
黒色コロイドMO,3
ゼラチン 1・0
紫外線吸収剤UV−10,1
同上 UV−20,1
同上 UV−30,1
分散オイル0il−L O,2同上 0
i1−2 0.1
第2層(中間層)
ゼラチン 1・0
カラードカプラーC−20,02
分散オイル 04l−10,01
第3層(低感度赤感性乳剤層)
単分散沃臭化銀乳剤(沃化銀3モル%、平均粒形1.
Oμ)1.8
ゼラチン 1.2増感色素1
1.4xlO−’増感色素口
7XIO−’カプラーC−10,5
カプラーC−20,05
分散オイル Of+−30,03
分散オイル 04l−40,03
第4層(中間層)
ゼラチン 1・ 0化合物7
1. 0. 1第5F!(低
感度緑感性乳剤層)
単分散沃臭化銀乳剤(沃化銀3モル%、平均粒形1.0
μ)1.4
(沃化銀3モル%、平均粒
形0.3μ)0.3
ゼラチン 0.8増感色素n
l 3X10−’増感色素rv
1xlO−’増感色素V
lXl0−’カプラーC−30,
7
カプラーC−40,1
カプラーC−50,1
分散オイル 041−30.1
第6層(中間層)
ゼラチン 1.0化合物A
0. 1第7層(低感度青
感性乳剤層)
単分散沃臭化銀乳剤(沃化銀3モル%、平均粒形1.0
μ)0.7
(沃化銀3モル%、平均粒
形0.3μ) 0゜2ゼラチン
1.0増感色素Vl
2xlO−’増感色素■
2 X 10−’カプラーC−60,9
カプラーC−100,2
分散オイル 0il−10,1
第8層(中間層)
ゼラチン 1.0化合物A
0. 1第9Jffl(高
感度赤感性乳剤rvJ)多分散沃臭化銀乳剤(沃化銀6
モル%、平均粒形2.0μ)2.3
ゼラチン 1.2増感色素+
7X10−’増感色素II
2X10−’カプラーC−8
0゜■
カプラーC−10,2
分散オイル 0il−40,2
第1O層(中間層)
ゼラチン 1. 。(Composition of photosensitive layer) First layer (antihalation layer) Black colloid MO,3 Gelatin 1.0 Ultraviolet absorber UV-10,1 Same as above UV-20,1 Same as above UV-30,1 Dispersion oil 0il-L O, 2 Same as above 0
i1-2 0.1 2nd layer (intermediate layer) Gelatin 1.0 Colored coupler C-20,02 Dispersion oil 04l-10,01 3rd layer (low sensitivity red-sensitive emulsion layer) Monodispersed silver iodobromide emulsion ( Silver iodide 3 mol%, average grain size 1.
Oμ) 1.8 Gelatin 1.2 Sensitizing dye 1
1.4xlO-' sensitizing dye port
7XIO-'Coupler C-10,5 Coupler C-20,05 Dispersion oil Of+-30,03 Dispersion oil 04l-40,03 4th layer (middle layer) Gelatin 1.0 Compound 7
1. 0. 1st 5th F! (Low-sensitivity green-sensitive emulsion layer) Monodispersed silver iodobromide emulsion (silver iodide 3 mol%, average grain size 1.0
μ) 1.4 (Silver iodide 3 mol%, average grain size 0.3 μ) 0.3 Gelatin 0.8 Sensitizing dye n
l 3X10-' sensitizing dye rv
1xlO-'sensitizing dye V
lXl0-' coupler C-30,
7 Coupler C-40.1 Coupler C-50.1 Dispersion oil 041-30.1 6th layer (middle layer) Gelatin 1.0 Compound A
0. 1 Seventh layer (low sensitivity blue-sensitive emulsion layer) Monodispersed silver iodobromide emulsion (silver iodide 3 mol%, average grain size 1.0
μ) 0.7 (Silver iodide 3 mol%, average grain size 0.3 μ) 0°2 gelatin
1.0 sensitizing dye Vl
2xlO-'sensitizing dye■
2
0. 1 No. 9 Jffl (high sensitivity red-sensitive emulsion rvJ) polydispersed silver iodobromide emulsion (silver iodide 6
Mol%, average particle size 2.0μ) 2.3 Gelatin 1.2 Sensitizing dye +
7X10-' Sensitizing Dye II
2X10-'Coupler C-8
0゜■ Coupler C-10,2 Dispersion oil 0il-40,2 1st O layer (intermediate layer) Gelatin 1. .
カプラーC−50・ 2
化合物A O・ l第11層
(高感度緑感性乳剤層)
多分散沃臭化銀乳剤(沃化銀5モル%、平均粒形2.
Oμ)2.0
ゼラチン 1.0増感色素1
[[I X 10−’
IV 3XIO−5V
3xlO−’カプラーC−90,2
分散オイル0i1−1 0.4第12暦(
中間層)
微粒子臭化銀乳剤(平均粒形0.07μ)2.0ゼラチ
ン 1・2
化合物A0.1
第13M(窩感度青感性乳剤層)
甲1分散沃臭化銀乳剤(沃化銀3モル%、平均粒形2.
1μ)1.8
中8分散沃臭化銀乳剤(沃化銀3モル%、平均粒形1.
2μ)0.5
単分散沃臭化銀乳剤(沃化銀3モル%、平均粒形0.3
μ)0.2
微粒子沃臭化銀乳剤(平均粒形0.09μ)0.2ゼラ
チン 1・2
増感色素VI 3X10−
’増感色素■ I X 10
−’カプラーC−60,3
分散オイル0il(0,06
第14層(第1保護NJ)
カプラーC−70,1
紫外線吸収剤UV−10,05
同上0v−z o、os
同上[IV−30,05
同上υV−40,05
同上UV−50,05
ゼラチン 0・6
分散オイル0il−40,1
第15層(第2保!!層)
ゼラチン 0.5
ポリメチルメタアクリレート粒子(直径1.5μ)各層
には上記成分の他に界面活性剤W−1,を塗布助剤とし
て添加した。更にホルマリンスカベンジャ−も添加した
。Coupler C-50.2 Compound A O.l 11th layer (high-sensitivity green-sensitive emulsion layer) Polydisperse silver iodobromide emulsion (silver iodide 5 mol%, average grain size 2.
Oμ) 2.0 Gelatin 1.0 Sensitizing dye 1
[[I X 10-' IV 3XIO-5V
3xlO-'Coupler C-90,2 Dispersion Oil 0i1-1 0.4 12th Calendar (
Intermediate layer) Fine-grain silver bromide emulsion (average grain size 0.07μ) 2.0 Gelatin 1.2 Compound A0.1 13M (fove-sensitive blue-sensitive emulsion layer) A1 dispersed silver iodobromide emulsion (silver iodide 3 Mol%, average particle shape2.
1μ) 1.8 medium 8-dispersed silver iodobromide emulsion (silver iodide 3 mol%, average grain size 1.8)
2μ) 0.5 Monodisperse silver iodobromide emulsion (silver iodide 3 mol%, average grain size 0.3
μ) 0.2 Fine grain silver iodobromide emulsion (average grain size 0.09μ) 0.2 Gelatin 1.2 Sensitizing dye VI 3X10-
'Sensitizing dye ■ I X 10
-'Coupler C-60,3 Dispersion oil 0il (0,06 14th layer (1st protection NJ) Coupler C-70,1 Ultraviolet absorber UV-10,05 Same as above 0v-z o, os Same as above [IV-30 ,05 Same as above υV-40,05 Same as above UV-50,05 Gelatin 0.6 Dispersion oil 0il-40,1 15th layer (2nd protection!! layer) Gelatin 0.5 Polymethyl methacrylate particles (diameter 1.5μ ) In addition to the above components, a surfactant W-1 was added as a coating aid to each layer.A formalin scavenger was also added.
なお、感光材料中への添加量は1イ当たり何グラムかを
示しており、又ハロゲン化銀乳剤とコロイド銀は銀に換
算して示し、増感色素はハロゲン化銀とのモル比で示し
た。The amount added to the light-sensitive material is shown in grams per 1 yen, silver halide emulsion and colloidal silver are shown in terms of silver, and sensitizing dyes are shown in molar ratio with silver halide. Ta.
実施例に使用した化合物 tc、H,工(し) C−2 杏ニ Q 曜 OCH,C0NHCH,CH,OCH。Compounds used in examples tc, H, engineering (shi) C-2 Anni Q day of the week OCH, CONHCH, CH, OCH.
増感色素I
同上 ■
同上 ■
同上 ■
同上 V
同上 ■
同上 ■
JV−1
V−2
V−3
V−4
V−5
化合物AW−1
試料101のカプラーを第1表のように変更する以外は
試料101と全く同様にして試料102〜108を作っ
た。ただしカプラーは等モル置き換えをした。Sensitizing dye I Same as above ■ Same as above ■ Same as above ■ Same as above V Same as above ■ Same as above ■ JV-1 V-2 V-3 V-4 V-5 Compound AW-1 Except for changing the coupler of sample 101 as shown in Table 1. Samples 102 to 108 were made in exactly the same manner as sample 101. However, the couplers were replaced equimolarly.
第1表
得られた試料101〜108を35m/m巾に裁断後、
標準的な被写体を撮影し、下記処理工程(+)を通して
各々500mのランニングテストをおこなった。After cutting the obtained samples 101 to 108 in Table 1 to a width of 35 m/m,
Standard subjects were photographed and a running test of 500 m was conducted for each subject through the following processing steps (+).
ランニング終了後試料〔O1〜108に5CMSの像様
露光を与え(1)の処理を行った。その後残留銀量を螢
光X線にて測定した。After the running was completed, the samples [O1 to 108] were subjected to imagewise exposure of 5 CMS and processed in (1). Thereafter, the amount of residual silver was measured using fluorescent X-rays.
上記処理工程において、水洗■、■、■は■−■−■へ
の向流方式とした。In the above treatment steps, water washing (1), (2), and (2) were carried out in a countercurrent manner to (■-■-■).
(発色現像液)
母 液(g) 補充液(g)
ジエチレントリアミン 1.0 1.2五酢酸
1−ヒドロキシエチリ
チン−1,1−ジ 2.0 2.4ホスホン酸
亜硫酸ナトリウム 2.0 4.8炭酸カリ
ウム 35.0 45.0臭化カリウム
I、6−
沃化カリウム 2.0mg −ヒドロキ
シルアミン 2.0 3.64−(N−エチ
ル−5,07,5
N−β−ヒドロキ
シエチルアミノ)
−2−メチルアニ
リン硫酸塩
水を加えて 12 11pH(水酸
化カリ 10. 20 10. 35ウムを用いて)
(漂白定着液)
母 液(g) 補充液(g)
エチレンジアミン四 40 45酢酸第2鉄
アンモ
ニウム塩
ジエチレントリアミ 40 45ン五酢酸
第2鉄ア
ンモニウム塩
エチレンジアミン 10 1〇四酢酸二ナ
トリウ
ム塩
亜硫酸ナトリウム 15 20チオ硫酸
アンモニウ 240 270ム水を8液(70
%
w / v )
アンモニア水(26%) 14mj! 12
mj!水を加えて 1j!
1NpH6,76,5
(水洗水)
以下の3種類を用いた。(Color developer) Mother solution (g) Replenisher (g) Diethylenetriamine 1.0 1.2 Pentaacetic acid 1-hydroxyethyritine-1,1-di 2.0 2.4 Sodium sulfite phosphonate 2.0 4. 8 Potassium carbonate 35.0 45.0 Potassium bromide
I, 6-Potassium iodide 2.0mg -Hydroxylamine 2.0 3.64-(N-ethyl-5,07,5N-β-hydroxyethylamino)-2-Methylaniline sulfate solution added 12 11pH (Using potassium hydroxide 10.20 10.35 um) (Bleach-fix solution) Mother solution (g) Replenisher (g) Ethylenediamine 40 45 ferric ammonium acetate diethylenetriamine 40 45 ferric pentaacetate Ammonium salt ethylenediamine 10 10 Tetraacetic acid disodium salt Sodium sulfite 15 20 Ammonium thiosulfate 240 270 ml water (8 solutions)
% w/v ) Ammonia water (26%) 14mj! 12
mj! Add water 1j!
1N pH 6,76,5 (washing water) The following three types were used.
(1)水道水
カルシウム 26 m g / f!マグネシ
ウム 9mg/l
pH7,2
(2)イオン交換処理水
三菱化成■製強酸性カチオン交換樹脂(Na形)を用い
て上記水道水を処理し、下記水質とした。(1) Tap water calcium 26 mg/f! Magnesium 9 mg/l pH 7.2 (2) Ion exchange treated water The above tap water was treated using a strongly acidic cation exchange resin (Na type) manufactured by Mitsubishi Kasei ■ to give the following water quality.
カルシウム 1.1mg/j!
マグネシウム 0.5mg/4
pH6,6
(3)キレート剤を添加した水道水
前記水道水に、エチレンジアミン四酢酸二ナトリウム塩
を500mg//!添加した。Calcium 1.1mg/j! Magnesium 0.5mg/4 pH 6,6 (3) Tap water with chelating agent added 500mg// of ethylenediaminetetraacetic acid disodium salt to the tap water! Added.
pH6,7 以上記載の如くの工程及び処理液にて、実施した。pH6,7 The experiment was carried out using the steps and treatment liquid as described above.
l(比較例) EXC−3EXC−6(1)
45 1(旧 65−
2(# ) # (37) (1
) 18 12(n) 23
−
3(l ) Cリ (37) (
+) 19 10(II) 2
5 −
4(−) # (2) (1
) 10 11(n) 19
−
5(本発明”) A−3(37) (1)
8 4(n) 17
−
6(〃 )A−5(37) (1)
9 5([1) 15
−7(〃 ) A−7(7) (1)
10 6(n) 1B
−8(1) A、−3(7) (+
) 8 3(旧 16 −
q(〃 ) A−3(15) (+)
9 4(II) 1B
−0(’) A−5(15) (
+) 9 5(旧 16
−
☆ 35m/m中1m当り
上記処理工程において、安定■、■、■は■→■→■へ
の向流方式とした。又、定着液の水洗タンクへの持ち込
み量は1m当り2mfであった。l (Comparative example) EXC-3EXC-6 (1)
45 1 (old 65-2 (#) # (37) (1
) 18 12(n) 23
−3(l) Cli (37) (
+) 19 10(II) 2
5 - 4(-) # (2) (1
) 10 11(n) 19
-5 (This invention”) A-3 (37) (1)
8 4(n) 17
-6(〃)A-5(37) (1)
9 5 ([1) 15
-7(〃) A-7(7) (1)
10 6(n) 1B
-8(1) A, -3(7) (+
) 8 3 (old 16-q(〃 ) A-3(15) (+)
9 4(II) 1B
-0(') A-5(15) (
+) 9 5 (old 16
- ☆ In the above treatment process per 1 m in 35 m/m, stable ■, ■, and ■ were conducted in a countercurrent direction from ■→■→■. Further, the amount of fixer carried into the washing tank was 2 mf/m.
(発色現像液)
母 液(g) 補充液(g)
ジエチレン 1.0 2.0トリアミ
ン五酢酸
1−ヒドロキシ 2.0 3.3エチリデ
ン−1゜
1−ジホスホン酸
亜硫酸ナトリウム 4.0 5.0炭酸カリ
ウム 30.0 38.0臭化カリウム
1.4 □沃化カリウム
1.3■ □ヒドロキシアミン 2.4
3.24−(N−エチル−4,57,2
N−β−ヒドロキシ
−エチルアミノ)−2−
メチルアニリン硫酸塩
水を加えて、 iz ij!p
H10,0010,05
(漂白液)
母液(g) 補充液(g)
エチレンジアミン四酢酸 50 60第2鉄アン
モニウム塩
1.3−ジアミノプロパ 60 72ン四酢酸第2
鉄アンモ
ニウム塩
アンモニア水 7m1 5mj!硝酸アン
モニウム 10.0g 12.0g臭化アンモ
ニウム 150g 170g水を加えて
1x 1j!pH6,05,8
(定着液)
母液(g) 補充液(g)
エチレンジアミン四酢酸 1.0 1.2二ナトリ
ウム塩
亜硫酸ナトリウム 4.0 5.0重亜硫酸
ナトリウム 4.6 5.8チオ硫酸アンモニ
ウム
水溶液(Toχ) 115m1 200m
j!水を加えて 11 11pH6
,66,6
(安定液)
母液(g) 補充液(g)
残留銀量を第3表に示した。(Color developer) Mother solution (g) Replenisher (g) Diethylene 1.0 2.0 Triaminepentaacetic acid 1-hydroxy 2.0 3.3 Ethylidene-1°1-diphosphonic acid sodium sulfite 4.0 5.0 Potassium carbonate 30.0 38.0 Potassium bromide
1.4 □ Potassium iodide
1.3■ □Hydroxyamine 2.4
3. Add 24-(N-ethyl-4,57,2 N-β-hydroxy-ethylamino)-2-methylaniline sulfate solution, iz ij! p
H10,0010,05 (Bleach solution) Mother liquor (g) Replenisher solution (g) Ethylenediaminetetraacetic acid 50 60 Ferric ammonium salt 1,3-diaminopropane 60 72Ntetraacetic acid 2
Iron ammonium salt ammonia water 7ml 5mj! Ammonium nitrate 10.0g 12.0g Ammonium bromide 150g 170g Add water
1x 1j! pH 6,05,8 (Fixer) Mother liquor (g) Replenisher (g) Ethylenediaminetetraacetic acid 1.0 1.2 Disodium salt Sodium sulfite 4.0 5.0 Sodium bisulfite 4.6 5.8 Ammonium thiosulfate aqueous solution (Toχ) 115m1 200m
j! Add water 11 11pH6
,66,6 (Stable solution) Mother liquor (g) Replenisher solution (g) The amount of residual silver is shown in Table 3.
第3表
以上の中で試料lO5,106,109は赤感層の感度
がやや減少しているのがみとめられたが、上記本発明の
試料は脱銀性が著るしく改善されているのがわかる。Among the samples in Table 3 and above, it was observed that the sensitivity of the red-sensitive layer was slightly decreased in Samples 1O5, 106, and 109, but the above-mentioned samples of the present invention had significantly improved desilvering properties. I understand.
実施例2
実施例1の試料101を変更して次の試料201を作っ
た。Example 2 Sample 101 of Example 1 was changed to produce the following sample 201.
第1N 試料101の 第1層と同じ
第2N 第2層 〃
第3層 第3層 I
第4層 第9層 〃
第5層 第4N 〃
第6層 第5層 〃
第7層 第6層 〃
第8層 第77W 〃
第9N 第8層 〃
第10i 第11層 〃第111
第12層 〃第12層
第13N〃
第13層 第14層 〃第14層
第15層 〃試料102に対しても同様なy
Z順の入れかえを行って試料202を作った。1N Same as the 1st layer of sample 101 2N 2nd layer 〃 3rd layer 3rd layer I 4th layer 9th layer 〃 5th layer 4N 〃 6th layer 5th layer 〃 7th layer 6th layer 〃 8th layer 77W 9N 8th layer 10i 11th layer 111
12th layer 〃12th layer
13th layer 13th layer 14th layer 14th layer
15th layer Same y for sample 102
Sample 202 was created by performing Z-order replacement.
試料101.102.201.202に実施例1と同様
な処理を施し、残留銀量と試料101の赤感層の感度を
100とした時の相対感度を求めた。その結果を表4に
示した。Samples 101, 102, 201, and 202 were subjected to the same treatment as in Example 1, and the amount of residual silver and the relative sensitivity when the sensitivity of the red-sensitive layer of sample 101 was set to 100 were determined. The results are shown in Table 4.
表 4
以上より本発明の層配列にて本発明の化合物を用いると
高感度を維持したまま脱銀が改良できることがわかった
。Table 4 From the above, it was found that when the compound of the present invention was used in the layer arrangement of the present invention, desilvering could be improved while maintaining high sensitivity.
実施例3
実施例1の試料101の乳剤層の乳剤の塗布量と粒子サ
イズを第5表のようにかえて試料301〜304を作っ
た。また試料102に対しても同様にして305〜30
8を作った。Example 3 Samples 301 to 304 were prepared by changing the emulsion coating amount and grain size of the emulsion layer of sample 101 of Example 1 as shown in Table 5. Similarly, for sample 102, 305 to 30
I made 8.
得られた試料301〜306を35mm巾にカット後、
標準的な被写体を撮影し、次の処理工程(n)を通して
各々500mのランニングテストを行った。After cutting the obtained samples 301 to 306 into 35 mm width,
Standard objects were photographed and each underwent a 500 m running test through the following processing step (n).
ランニング終了後、試料301〜308に50M5の像
様露光を与え、その後(n)の処理を行い残留銀量の測
定を行った。残留銀量は、最大露光部で行った。その結
果を第6表に示した。After the running was completed, samples 301 to 308 were subjected to imagewise exposure of 50M5, and then subjected to the process (n) to measure the amount of residual silver. The amount of residual silver was measured at the maximum exposure area. The results are shown in Table 6.
第5表
処理工程(■) (温度38℃)☆ 35m/
m中1m当り
上記処理工程において、安定■、■、■は■−■−■へ
の向流方式とした。又、定着液の水洗タンクへの持ち込
み量は1m当り2ml!であった。Table 5 Treatment process (■) (Temperature 38℃)☆ 35m/
In the above-mentioned treatment steps, stable (1), (2), and (2) were conducted in a countercurrent manner to (1) - (2) - (2). Also, the amount of fixer to be carried into the washing tank is 2ml per 1m! Met.
(発色現像液)
母液軸) 補充液(g)
ジエチレントリアミン L、0 2.0五酢酸
■−ヒドロキシエチリ 2.0 3.3デンー1
.1−ジホ
スホン酸
亜硫酸ナトリウム 4.0 5.0炭酸カリウ
ム 30.0 3B、0臭化カリウム
1.4 □沃化カリウム 1.3■
□ヒドロキシアミン 2.4 3.24−(
N−エチル−N 4.5 7.2−β−ヒドロキシエ
チルアミノ)−2−
メチルアニリン硫酸塩
水を加えて 1z IzpH1
0,0010,05
(漂白液)
母液(g) 補充液(g)
エチレンジアミン四節 50 60酸第2鉄ア
ンモニウ
ム塩
1.3−ジアミノプロ 60 72パン四酢酸
第2鉄ア
ンモニウム塩
アンモニア水 7m/ 5mn硝酸ア
ンモニウム 10.0g ’ 12.0g臭化
アンモニウム 150g 170g水を加えて
11 lI!。(Color developer) Mother liquid axis) Replenisher (g) Diethylenetriamine L, 0 2.0 Pentaacetic acid ■-Hydroxyethyl 2.0 3.3 Den-1
.. 1-diphosphonic acid sodium sulfite 4.0 5.0 Potassium carbonate 30.0 3B, 0 Potassium bromide
1.4 □Potassium iodide 1.3■
□Hydroxyamine 2.4 3.24-(
N-ethyl-N 4.5 7.2-β-hydroxyethylamino)-2- Add methylaniline sulfate solution 1z IzpH1
0,0010,05 (Bleach solution) Mother liquor (g) Replenisher (g) Ethylenediamine tetrahedron 50 60 acid ferric ammonium salt 1,3-diaminopro 60 72 Pantetraacetic acid ferric ammonium salt Aqueous ammonia 7m/5mn Ammonium nitrate 10.0g ' 12.0g Ammonium bromide 150g 170g Add water 11 lI! .
pH6,05,8
(定着液)
母液(g) 補充液(g)
エチレンジアミン四節 1.0 1.2酸二ナトリ
ウム塩
亜硫酸ナトリウム 4.0 5.0重亜硫酸ナ
トリウム 4.6 5.8チオ硫酸アンモニウム
水溶液(70%) 175m l! 20
0m l水を加えて 11 11p
H6,66,6
(安定液)
母液(g) 補充液(g)
ホルマリン
(37%W / V ) 2.0 m 1
3.0 m lポリオキシエチレン 0.3 0
.45−p−モノノニル
フェニルエーテル
(平均重合度10)
5−クロロ−2−メチ 0.03 0.045ルー
4−イソチアゾ
リン−3−オン
水を加えて 11 1x第6表
以上より本発明の効果は銀量が多い程著るしく1E14
it5.8g/fflの試料では効果は認められるが差
が小さくなっていることがわかる。pH 6,05,8 (Fixer) Mother liquor (g) Replenisher (g) Ethylenediamine 1.0 1.2 acid disodium salt Sodium sulfite 4.0 5.0 Sodium bisulfite 4.6 5.8 Ammonium thiosulfate Aqueous solution (70%) 175ml! 20
Add 0ml water 11 11p
H6,66,6 (stable solution) Mother liquor (g) Replenisher solution (g) Formalin (37% W/V) 2.0 m 1
3.0 ml polyoxyethylene 0.3 0
.. 45-p-monononylphenyl ether (average degree of polymerization 10) 5-chloro-2-methy 0.03 0.045 4-isothiazolin-3-one Add water 11 1x From Table 6 and above, the effects of the present invention 1E14 becomes more pronounced as the amount of silver increases.
It can be seen that in the sample with it5.8g/ffl, although the effect is recognized, the difference is smaller.
実施例4
下塗りをした三酢酸セルロースフィルム支持体上に、下
記に示すような組成の各層よりなる多層カラー感光材料
である試料401を作成した。Example 4 Sample 401, which is a multilayer color photosensitive material, was prepared on a subbed cellulose triacetate film support, each layer having the composition shown below.
□ 第1層(ハレーション防止N)
黒色コロイド銀 0.3ゼラチン
1.0紫外線吸収剤 UV
−1’0.1
同上 UV−20、l
同上 UV−30,1
分散オイル 0il−10,2
同上 0il−20,1
第2層(中間層)
ゼラチン 1.0カラードカ
プラーC−10,02
分散オイル Of!−10,01
第3層(低感度赤感性乳剤層)
単分散沃臭化銀乳剤(沃化銀8モル%、平均粒形1.0
μ)1.4
ゼラチン 1.1増感色素1
1.4X10−’増感色素■
7X10−’カプラーC−20,5
カプラーC−30,05
カプラーC−40,05
分散オイル 0il−30,03
分散オイル 041−40.03
第47W(中間N)
ゼラチン 1.0分散オイル
0in−10,05
カプラーC−50,15
第5N(低感度緑感性乳剤層)
単分散沃臭化銀乳剤(沃化銀8モル%、平均粒形1.0
μ)1.5
(沃化銀3モル%、平均粒
形0.3μ)0.3
ゼラチン 0.8増感色素[
13X10−’
増感色素rV 1xlO−’増
感色素V lXl0−’”
V[lXl0−’
カプラーC−60,4
カプラーC−10,1
分散オイル 0il−30,1
第6N(中間層)
ゼラチン 1.0分散オイル
01e−10,05
カプラーC−50,15
第7層(低感度青感性乳剤層)
単分散沃臭化銀乳剤(沃化銀8モル%、平均粒形1.0
μ)0.9
ゼラチン 1.0増感色素■
2X10−’増感色素■
2X10−’カプラーC−70,9
分散オイル Of!−10,1
第8層(中間層)
ゼラチン 1.0カプラーC
−50,15
第9層(高感度緑感性乳剤N)
沃臭化銀乳剤(沃化!15.5モル、平均粒径2.0μ
)2.1
(〃 8モル、 平均粒径
1.2μ)0.8
(〃 2.5モル、平均粒径
0.5μ)0.3
ゼラチン 1.2増感色素(
7xlO−’
増感色素u 2X10−’カプ
ラーC−80,1
カプラーC−40,2
分散オイル Oi+−40,2
第10層(中間層)
ゼラチン 1. 0カプラー
C−50,1
第11層(高感度緑感性乳剤N)
沃臭化銀乳剤(沃化銀5.5モル%、平均粒形2、0μ
)1.2
(〃 8モル%、 平均粒径
1.0μ)0.8
ゼラチン 1.0増感色素m
1.5X10−’” IV
5X10−’” V
5X10−’“ Vl
5xio−’’ EX
lXl0−’カプラーC−60.2
カプラーC−10,05
分散オイル Oi+−10,4
第12N(中間層)
微粒子臭化銀乳剤(平均粒形0.07μ)2.0
ゼラチン 1. 2分散オイ
ル oil−10,05
カプラーC−50,1
第13N(高感度青感性乳剤層)
単分散沃臭化銀乳剤(沃化銀6モル%、平均粒形2.1
μ)1.8
単分散沃臭化銀乳剤(沃化銀8モル%、平均粒形1.2
μ)0.5
単分散沃臭化銀乳剤(沃化銀3モル%、平均粒形0.3
μ)0.2
微粒子沃臭化銀乳剤(平均粒形0.09μ)0.2
ゼラチン 1.2増感色素■
3X10−’増感色素■
lXl0−’カプラーC−7Q、
3
分散オイル 01l−10,06
第14層(第1保!i層)
紫外線吸収剤 tJV−10,05
同上 UV−20,05
同上 UV−30,05
同上 UV−40,05
同上 UV−50,05
ゼラチン 0.6分散オイル
01m−40,1
第15層(第2保護層)
ゼラチン 0.5ポリメチル
メタアクリレ一ト粒子(直径1.5μ)各層には上記成
分の他に界面活性剤WA−1を全体で0.25.、硬膜
剤+1−1を0.4g使用した。更にホルマリンスカベ
ンジャ−も添加した。□ 1st layer (antihalation N) Black colloidal silver 0.3 Gelatin 1.0 Ultraviolet absorber UV
-1'0.1 Same as above UV-20, l Same as above UV-30,1 Dispersion oil 0il-10,2 Same as above 0il-20,1 2nd layer (intermediate layer) Gelatin 1.0 Colored coupler C-10,02 Dispersion Oil Of! -10,01 Third layer (low sensitivity red-sensitive emulsion layer) Monodispersed silver iodobromide emulsion (silver iodide 8 mol%, average grain size 1.0
μ) 1.4 Gelatin 1.1 Sensitizing dye 1
1.4X10-'sensitizing dye■
7X10-' Coupler C-20,5 Coupler C-30,05 Coupler C-40,05 Dispersion oil 0il-30,03 Dispersion oil 041-40.03 No. 47W (Intermediate N) Gelatin 1.0 Dispersion oil 0in-10 ,05 Coupler C-50,15 5th N (low-sensitivity green-sensitive emulsion layer) Monodisperse silver iodobromide emulsion (silver iodide 8 mol%, average grain size 1.0
μ) 1.5 (Silver iodide 3 mol%, average grain size 0.3 μ) 0.3 Gelatin 0.8 Sensitizing dye [
13X10-' Sensitizing dye rV 1xlO-' Sensitizing dye V lXl0-'
V[lXl0-' Coupler C-60,4 Coupler C-10,1 Dispersion oil 0il-30,1 6th N (intermediate layer) Gelatin 1.0 Dispersion oil 01e-10,05 Coupler C-50,15 7th layer (Low sensitivity blue-sensitive emulsion layer) Monodisperse silver iodobromide emulsion (silver iodide 8 mol%, average grain size 1.0
μ) 0.9 Gelatin 1.0 Sensitizing dye■
2X10-'sensitizing dye■
2X10-'Coupler C-70,9 Dispersion Oil Of! -10,1 8th layer (middle layer) Gelatin 1.0 Coupler C
-50,15 9th layer (high sensitivity green-sensitive emulsion N) Silver iodobromide emulsion (iodide! 15.5 mol, average grain size 2.0μ
) 2.1 (〃 8 mol, average particle size 1.2 μ) 0.8 (〃 2.5 mol, average particle size 0.5 μ) 0.3 Gelatin 1.2 Sensitizing dye (
7xlO-' Sensitizing dye u 2X10-' Coupler C-80,1 Coupler C-40,2 Dispersion oil Oi+-40,2 10th layer (intermediate layer) Gelatin 1. 0 coupler C-50,1 11th layer (high sensitivity green-sensitive emulsion N) Silver iodobromide emulsion (silver iodide 5.5 mol%, average grain size 2, 0μ
) 1.2 (〃 8 mol%, average particle size 1.0μ) 0.8 Gelatin 1.0 Sensitizing dye m
1.5X10-'” IV
5X10-'”V
5X10-'“Vl
5xio-''EX
lXl0-'Coupler C-60.2 Coupler C-10,05 Dispersion oil Oi+-10,4 12th N (intermediate layer) Fine grain silver bromide emulsion (average grain size 0.07μ) 2.0 Gelatin 1. 2 Dispersion oil oil-10,05 Coupler C-50,1 13th N (high sensitivity blue-sensitive emulsion layer) Monodisperse silver iodobromide emulsion (silver iodide 6 mol%, average grain size 2.1
μ) 1.8 Monodisperse silver iodobromide emulsion (silver iodide 8 mol%, average grain size 1.2
μ) 0.5 Monodisperse silver iodobromide emulsion (silver iodide 3 mol%, average grain size 0.3
μ) 0.2 Fine grain silver iodobromide emulsion (average grain size 0.09 μ) 0.2 Gelatin 1.2 Sensitizing dye■
3X10-'sensitizing dye■
lXl0-' coupler C-7Q,
3 Dispersion oil 01l-10,06 14th layer (1st protection! i layer) Ultraviolet absorber tJV-10,05 Same as above UV-20,05 Same as above UV-30,05 Same as above UV-40,05 Same as above UV-50, 05 Gelatin 0.6 Dispersion oil 01m-40,1 15th layer (second protective layer) Gelatin 0.5 Polymethyl methacrylate particles (diameter 1.5μ) Each layer contains surfactant in addition to the above ingredients WA-1 as a whole is 0.25. , 0.4 g of hardener +1-1 was used. Additionally, formalin scavenger was added.
各層には上記成分の他に界面活性7FllW−1を塗布
助剤として添加した。更にホルマリンスカベンジャ−も
添加した。In addition to the above components, surfactant 7FllW-1 was added to each layer as a coating aid. Additionally, formalin scavenger was added.
なお、感光材料中への添加量はl−当たり何グラムかを
示しており、又ハロゲン化銀乳剤とコロイド銀は銀に換
算して示し、増感色素はハロゲン化銀とのモル比で示し
た。The amount added to the light-sensitive material is shown in grams per liter, silver halide emulsion and colloidal silver are shown in terms of silver, and sensitizing dyes are shown in molar ratio with silver halide. Ta.
実施例に使用した化合物
UV−3
C*Hs
−I
C−3
C−61(
同 上 ■
zHs
同 上 ■
z HS
(CHJa SOie(CHz)n 503 Na同
上 V
同 上 ■
同 上 ■
(CHx)+ 5O3e(CHJz SOs Na同上
■′
同上■
i 1−1
CHz =CHSot CHz
CHz =CHSCh CHz
A−1
この試料を用いて実施例1と同様な変更を行い、実施例
1と同様な処理を行ったところ、実施例1と同様な結果
を得、本発明の効果が確認できた。Compounds used in Examples UV-3 C*Hs -I C-3 C-61 (same as above ■ zHs same as above ■ z HS (CHJa SOie (CHz) n 503 Na same)
V Same as above ■ Same as above ■ (CHx) + 5O3e (CHJz SOs Na Same as above ■' Same as above ■ i 1-1 CHz =CHSot CHz CHz =CHSCh CHz A-1 Using this sample, the same changes as in Example 1 were made. When the same treatment as in Example 1 was carried out, the same results as in Example 1 were obtained, confirming the effect of the present invention.
特許出願人 富士写真フィルム株式会社昭和63年/月
4日Patent applicant: Fuji Photo Film Co., Ltd. April 4, 1986
Claims (1)
を有し、これらのうち少くとも1つが互いに感度の異な
る2つ以上の層からなり、この2層以上の層は支持体側
からみて低感層から高感層へと順に配列され、該低感層
と高感層の間に感色性の異なるハロゲン化銀乳剤層が少
くとも1つ配されているカラー感光材料が、芳香族第1
級アミン現像主薬の酸化体と反応して漂白促進剤を放出
する化合物を少くとも一種含有することを特徴とするハ
ロゲン化銀カラー感光材料。It has a blue-sensitive layer, a green-sensitive layer, and a red-sensitive silver halide emulsion layer, at least one of which is composed of two or more layers having mutually different sensitivities, and these two or more layers are on the support side. A color photosensitive material is arranged in order from a low-sensitivity layer to a high-sensitivity layer when viewed from above, and at least one silver halide emulsion layer having different color sensitivity is arranged between the low-sensitivity layer and the high-sensitivity layer, aromatic first
1. A silver halide color photosensitive material containing at least one compound that reacts with an oxidized product of a grade amine developing agent to release a bleaching accelerator.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP5128688A JPH01224755A (en) | 1988-03-04 | 1988-03-04 | Silver halide color photosensitive material |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP5128688A JPH01224755A (en) | 1988-03-04 | 1988-03-04 | Silver halide color photosensitive material |
Publications (1)
Publication Number | Publication Date |
---|---|
JPH01224755A true JPH01224755A (en) | 1989-09-07 |
Family
ID=12882687
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP5128688A Pending JPH01224755A (en) | 1988-03-04 | 1988-03-04 | Silver halide color photosensitive material |
Country Status (1)
Country | Link |
---|---|
JP (1) | JPH01224755A (en) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5561031A (en) * | 1995-03-23 | 1996-10-01 | Eastman Kodak Company | Color reversal elements with incorporated bleach accelerator |
-
1988
- 1988-03-04 JP JP5128688A patent/JPH01224755A/en active Pending
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5561031A (en) * | 1995-03-23 | 1996-10-01 | Eastman Kodak Company | Color reversal elements with incorporated bleach accelerator |
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