EP0871065A1 - Verarbeitungsverfahren für ein lichtempfindliches, photographisches Silberhalogenidfarbmaterial - Google Patents
Verarbeitungsverfahren für ein lichtempfindliches, photographisches Silberhalogenidfarbmaterial Download PDFInfo
- Publication number
- EP0871065A1 EP0871065A1 EP98106286A EP98106286A EP0871065A1 EP 0871065 A1 EP0871065 A1 EP 0871065A1 EP 98106286 A EP98106286 A EP 98106286A EP 98106286 A EP98106286 A EP 98106286A EP 0871065 A1 EP0871065 A1 EP 0871065A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- bleaching
- solution
- acid
- processing
- light
- 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.)
- Granted
Links
- -1 silver halide Chemical class 0.000 title claims abstract description 214
- 239000000463 material Substances 0.000 title claims abstract description 150
- 238000012545 processing Methods 0.000 title claims abstract description 142
- 229910052709 silver Inorganic materials 0.000 title claims abstract description 120
- 239000004332 silver Substances 0.000 title claims abstract description 120
- 238000000034 method Methods 0.000 title claims abstract description 73
- 238000004061 bleaching Methods 0.000 claims abstract description 198
- 150000001875 compounds Chemical class 0.000 claims abstract description 150
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 110
- 238000011161 development Methods 0.000 claims abstract description 45
- 150000003839 salts Chemical class 0.000 claims abstract description 32
- 239000002253 acid Substances 0.000 claims abstract description 30
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims abstract description 30
- 125000003118 aryl group Chemical group 0.000 claims abstract description 19
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 claims abstract description 14
- 125000000623 heterocyclic group Chemical group 0.000 claims abstract description 12
- 125000001931 aliphatic group Chemical group 0.000 claims abstract description 11
- 125000002947 alkylene group Chemical group 0.000 claims abstract description 11
- 150000001768 cations Chemical class 0.000 claims abstract description 11
- 238000005406 washing Methods 0.000 claims description 58
- 239000007844 bleaching agent Substances 0.000 claims description 36
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 claims description 17
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims description 13
- DMQQXDPCRUGSQB-UHFFFAOYSA-N 2-[3-[bis(carboxymethyl)amino]propyl-(carboxymethyl)amino]acetic acid Chemical compound OC(=O)CN(CC(O)=O)CCCN(CC(O)=O)CC(O)=O DMQQXDPCRUGSQB-UHFFFAOYSA-N 0.000 claims description 12
- SIOXPEMLGUPBBT-UHFFFAOYSA-N picolinic acid Chemical class OC(=O)C1=CC=CC=N1 SIOXPEMLGUPBBT-UHFFFAOYSA-N 0.000 claims description 11
- DIORMHZUUKOISG-UHFFFAOYSA-N sulfoformic acid Chemical compound OC(=O)S(O)(=O)=O DIORMHZUUKOISG-UHFFFAOYSA-N 0.000 claims description 5
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 claims description 4
- 230000008929 regeneration Effects 0.000 abstract description 26
- 238000011069 regeneration method Methods 0.000 abstract description 26
- 230000005587 bubbling Effects 0.000 abstract description 14
- 230000002829 reductive effect Effects 0.000 abstract description 12
- 239000000243 solution Substances 0.000 description 256
- 239000010410 layer Substances 0.000 description 150
- 239000000839 emulsion Substances 0.000 description 105
- 235000013339 cereals Nutrition 0.000 description 67
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 50
- 125000004432 carbon atom Chemical group C* 0.000 description 49
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 47
- 235000002639 sodium chloride Nutrition 0.000 description 41
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 40
- 229910001868 water Inorganic materials 0.000 description 40
- 239000000975 dye Substances 0.000 description 36
- 108010010803 Gelatin Proteins 0.000 description 35
- 229920000159 gelatin Polymers 0.000 description 35
- 235000019322 gelatine Nutrition 0.000 description 35
- 235000011852 gelatine desserts Nutrition 0.000 description 35
- 239000008273 gelatin Substances 0.000 description 34
- 239000002585 base Substances 0.000 description 31
- 239000000203 mixture Substances 0.000 description 31
- 239000004094 surface-active agent Substances 0.000 description 30
- 239000011248 coating agent Substances 0.000 description 29
- 238000000576 coating method Methods 0.000 description 29
- 230000018109 developmental process Effects 0.000 description 29
- 230000000087 stabilizing effect Effects 0.000 description 29
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 27
- 230000000694 effects Effects 0.000 description 25
- 230000001172 regenerating effect Effects 0.000 description 22
- 239000003381 stabilizer Substances 0.000 description 22
- 239000006096 absorbing agent Substances 0.000 description 21
- 125000000217 alkyl group Chemical group 0.000 description 21
- IOLCXVTUBQKXJR-UHFFFAOYSA-M potassium bromide Chemical compound [K+].[Br-] IOLCXVTUBQKXJR-UHFFFAOYSA-M 0.000 description 21
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 19
- 230000005291 magnetic effect Effects 0.000 description 19
- ZUNKMNLKJXRCDM-UHFFFAOYSA-N silver bromoiodide Chemical compound [Ag].IBr ZUNKMNLKJXRCDM-UHFFFAOYSA-N 0.000 description 18
- 239000006081 fluorescent whitening agent Substances 0.000 description 17
- 125000001424 substituent group Chemical group 0.000 description 16
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 15
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 15
- 238000001556 precipitation Methods 0.000 description 15
- 229910052783 alkali metal Inorganic materials 0.000 description 14
- 238000001035 drying Methods 0.000 description 14
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 14
- 239000002904 solvent Substances 0.000 description 14
- 238000005273 aeration Methods 0.000 description 13
- 239000006185 dispersion Substances 0.000 description 13
- 239000011347 resin Substances 0.000 description 13
- 229920005989 resin Polymers 0.000 description 13
- 239000011230 binding agent Substances 0.000 description 12
- 239000003755 preservative agent Substances 0.000 description 12
- 238000011282 treatment Methods 0.000 description 12
- 239000002738 chelating agent Substances 0.000 description 11
- 238000002156 mixing Methods 0.000 description 11
- 239000002245 particle Substances 0.000 description 11
- 229920000728 polyester Polymers 0.000 description 11
- 229920000642 polymer Polymers 0.000 description 11
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 11
- 230000001235 sensitizing effect Effects 0.000 description 11
- 239000000126 substance Substances 0.000 description 11
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 10
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 10
- 229910021607 Silver chloride Inorganic materials 0.000 description 10
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 10
- KDYFGRWQOYBRFD-UHFFFAOYSA-N Succinic acid Natural products OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 description 10
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 10
- 235000010724 Wisteria floribunda Nutrition 0.000 description 10
- 125000003342 alkenyl group Chemical group 0.000 description 10
- 235000011114 ammonium hydroxide Nutrition 0.000 description 10
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 10
- 239000006224 matting agent Substances 0.000 description 10
- JHJLBTNAGRQEKS-UHFFFAOYSA-M sodium bromide Chemical compound [Na+].[Br-] JHJLBTNAGRQEKS-UHFFFAOYSA-M 0.000 description 10
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 9
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 9
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 9
- 229910021612 Silver iodide Inorganic materials 0.000 description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- 235000011054 acetic acid Nutrition 0.000 description 9
- 150000003863 ammonium salts Chemical class 0.000 description 9
- 239000000872 buffer Substances 0.000 description 9
- 239000003112 inhibitor Substances 0.000 description 9
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 9
- 150000007524 organic acids Chemical class 0.000 description 9
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 9
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 8
- AEMRFAOFKBGASW-UHFFFAOYSA-N Glycolic acid Chemical compound OCC(O)=O AEMRFAOFKBGASW-UHFFFAOYSA-N 0.000 description 8
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 8
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 8
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 8
- SJOOOZPMQAWAOP-UHFFFAOYSA-N [Ag].BrCl Chemical compound [Ag].BrCl SJOOOZPMQAWAOP-UHFFFAOYSA-N 0.000 description 8
- 150000001340 alkali metals Chemical class 0.000 description 8
- 125000003545 alkoxy group Chemical group 0.000 description 8
- 238000009826 distribution Methods 0.000 description 8
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 8
- 238000002474 experimental method Methods 0.000 description 8
- 239000010419 fine particle Substances 0.000 description 8
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 description 8
- 230000003647 oxidation Effects 0.000 description 8
- 238000007254 oxidation reaction Methods 0.000 description 8
- 238000002360 preparation method Methods 0.000 description 8
- ADZWSOLPGZMUMY-UHFFFAOYSA-M silver bromide Chemical compound [Ag]Br ADZWSOLPGZMUMY-UHFFFAOYSA-M 0.000 description 8
- 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 7
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 description 7
- 239000002216 antistatic agent Substances 0.000 description 7
- 230000015572 biosynthetic process Effects 0.000 description 7
- 239000006249 magnetic particle Substances 0.000 description 7
- 229940045105 silver iodide Drugs 0.000 description 7
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 description 7
- 239000007787 solid Substances 0.000 description 7
- 239000002699 waste material Substances 0.000 description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 6
- DBVJJBKOTRCVKF-UHFFFAOYSA-N Etidronic acid Chemical compound OP(=O)(O)C(O)(C)P(O)(O)=O DBVJJBKOTRCVKF-UHFFFAOYSA-N 0.000 description 6
- 239000004698 Polyethylene Substances 0.000 description 6
- 238000007664 blowing Methods 0.000 description 6
- 239000000084 colloidal system Substances 0.000 description 6
- 239000000986 disperse dye Substances 0.000 description 6
- 230000005294 ferromagnetic effect Effects 0.000 description 6
- 230000006870 function Effects 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 6
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 description 6
- 239000012948 isocyanate Substances 0.000 description 6
- 150000002513 isocyanates Chemical class 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
- 229920003023 plastic Polymers 0.000 description 6
- 239000004033 plastic Substances 0.000 description 6
- 229920000573 polyethylene Polymers 0.000 description 6
- 238000006116 polymerization reaction Methods 0.000 description 6
- 229910000027 potassium carbonate Inorganic materials 0.000 description 6
- 235000011181 potassium carbonates Nutrition 0.000 description 6
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 description 6
- 239000000377 silicon dioxide Substances 0.000 description 6
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 6
- 125000000547 substituted alkyl group Chemical group 0.000 description 6
- BUUPQKDIAURBJP-UHFFFAOYSA-N sulfinic acid Chemical compound OS=O BUUPQKDIAURBJP-UHFFFAOYSA-N 0.000 description 6
- 125000000020 sulfo group Chemical group O=S(=O)([*])O[H] 0.000 description 6
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 6
- YXMWGHKZTMANIJ-UHFFFAOYSA-N 1h-pyrrol-2-ylmethanamine Chemical class NCC1=CC=CN1 YXMWGHKZTMANIJ-UHFFFAOYSA-N 0.000 description 5
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 description 5
- QPCDCPDFJACHGM-UHFFFAOYSA-N N,N-bis{2-[bis(carboxymethyl)amino]ethyl}glycine Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(=O)O)CCN(CC(O)=O)CC(O)=O QPCDCPDFJACHGM-UHFFFAOYSA-N 0.000 description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 5
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 description 5
- 239000000654 additive Substances 0.000 description 5
- SWLVFNYSXGMGBS-UHFFFAOYSA-N ammonium bromide Chemical compound [NH4+].[Br-] SWLVFNYSXGMGBS-UHFFFAOYSA-N 0.000 description 5
- XYXNTHIYBIDHGM-UHFFFAOYSA-N ammonium thiosulfate Chemical compound [NH4+].[NH4+].[O-]S([O-])(=O)=S XYXNTHIYBIDHGM-UHFFFAOYSA-N 0.000 description 5
- 125000000129 anionic group Chemical group 0.000 description 5
- 230000000844 anti-bacterial effect Effects 0.000 description 5
- DMSMPAJRVJJAGA-UHFFFAOYSA-N benzo[d]isothiazol-3-one Chemical compound C1=CC=C2C(=O)NSC2=C1 DMSMPAJRVJJAGA-UHFFFAOYSA-N 0.000 description 5
- 229910021538 borax Inorganic materials 0.000 description 5
- 230000001276 controlling effect Effects 0.000 description 5
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 5
- 229910052737 gold Inorganic materials 0.000 description 5
- 239000010931 gold Substances 0.000 description 5
- 150000002443 hydroxylamines Chemical class 0.000 description 5
- 150000004698 iron complex Chemical class 0.000 description 5
- 239000007788 liquid Substances 0.000 description 5
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 description 5
- 239000011976 maleic acid Substances 0.000 description 5
- 229910017604 nitric acid Inorganic materials 0.000 description 5
- 239000007800 oxidant agent Substances 0.000 description 5
- 229960003330 pentetic acid Drugs 0.000 description 5
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 5
- 239000001103 potassium chloride Substances 0.000 description 5
- 235000011164 potassium chloride Nutrition 0.000 description 5
- 238000003672 processing method Methods 0.000 description 5
- 230000009467 reduction Effects 0.000 description 5
- 238000006722 reduction reaction Methods 0.000 description 5
- 239000011734 sodium Substances 0.000 description 5
- 229910052708 sodium Inorganic materials 0.000 description 5
- 239000011780 sodium chloride Substances 0.000 description 5
- 235000010339 sodium tetraborate Nutrition 0.000 description 5
- 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 4
- AVXURJPOCDRRFD-UHFFFAOYSA-N Hydroxylamine Chemical compound ON AVXURJPOCDRRFD-UHFFFAOYSA-N 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 4
- 206010070834 Sensitisation Diseases 0.000 description 4
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 4
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 4
- 125000004183 alkoxy alkyl group Chemical group 0.000 description 4
- 125000000304 alkynyl group Chemical group 0.000 description 4
- 150000001412 amines Chemical class 0.000 description 4
- 125000004397 aminosulfonyl group Chemical group NS(=O)(=O)* 0.000 description 4
- 229910021529 ammonia Inorganic materials 0.000 description 4
- 235000019270 ammonium chloride Nutrition 0.000 description 4
- 239000003957 anion exchange resin Substances 0.000 description 4
- 239000011575 calcium Substances 0.000 description 4
- 125000003917 carbamoyl group Chemical group [H]N([H])C(*)=O 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 4
- 150000001735 carboxylic acids Chemical class 0.000 description 4
- 125000002057 carboxymethyl group Chemical group [H]OC(=O)C([H])([H])[*] 0.000 description 4
- 229920002678 cellulose Polymers 0.000 description 4
- 239000001913 cellulose Substances 0.000 description 4
- 239000002131 composite material Substances 0.000 description 4
- 230000003247 decreasing effect Effects 0.000 description 4
- 230000008021 deposition Effects 0.000 description 4
- 208000028659 discharge Diseases 0.000 description 4
- 238000001704 evaporation Methods 0.000 description 4
- 230000008020 evaporation Effects 0.000 description 4
- 229910052736 halogen Inorganic materials 0.000 description 4
- 150000002367 halogens Chemical class 0.000 description 4
- 239000004312 hexamethylene tetramine Substances 0.000 description 4
- 235000010299 hexamethylene tetramine Nutrition 0.000 description 4
- 230000001965 increasing effect Effects 0.000 description 4
- 229910052742 iron Inorganic materials 0.000 description 4
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 description 4
- 239000004816 latex Substances 0.000 description 4
- 229920000126 latex Polymers 0.000 description 4
- 125000000325 methylidene group Chemical group [H]C([H])=* 0.000 description 4
- 239000010413 mother solution Substances 0.000 description 4
- 150000002894 organic compounds Chemical class 0.000 description 4
- 239000003960 organic solvent Substances 0.000 description 4
- 230000001590 oxidative effect Effects 0.000 description 4
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 4
- 150000004989 p-phenylenediamines Chemical class 0.000 description 4
- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical compound OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 description 4
- 239000004848 polyfunctional curative Substances 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 239000011241 protective layer Substances 0.000 description 4
- 125000004076 pyridyl group Chemical group 0.000 description 4
- QEIQICVPDMCDHG-UHFFFAOYSA-N pyrrolo[2,3-d]triazole Chemical class N1=NC2=CC=NC2=N1 QEIQICVPDMCDHG-UHFFFAOYSA-N 0.000 description 4
- 150000003242 quaternary ammonium salts Chemical class 0.000 description 4
- 230000001603 reducing effect Effects 0.000 description 4
- YGSDEFSMJLZEOE-UHFFFAOYSA-N salicylic acid Chemical class OC(=O)C1=CC=CC=C1O YGSDEFSMJLZEOE-UHFFFAOYSA-N 0.000 description 4
- 230000008313 sensitization Effects 0.000 description 4
- UQDJGEHQDNVPGU-UHFFFAOYSA-N serine phosphoethanolamine Chemical compound [NH3+]CCOP([O-])(=O)OCC([NH3+])C([O-])=O UQDJGEHQDNVPGU-UHFFFAOYSA-N 0.000 description 4
- 229910000029 sodium carbonate Inorganic materials 0.000 description 4
- 235000017550 sodium carbonate Nutrition 0.000 description 4
- 239000001488 sodium phosphate Substances 0.000 description 4
- 235000010265 sodium sulphite Nutrition 0.000 description 4
- 239000004328 sodium tetraborate Substances 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
- 239000001384 succinic acid Substances 0.000 description 4
- LSNNMFCWUKXFEE-UHFFFAOYSA-L sulfite Chemical class [O-]S([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-L 0.000 description 4
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 description 4
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 4
- 150000003852 triazoles Chemical class 0.000 description 4
- 229920002554 vinyl polymer Polymers 0.000 description 4
- 229910000859 α-Fe Inorganic materials 0.000 description 4
- WHFGLPOOBLVZRM-UHFFFAOYSA-N 1,4-bis(1,2,4-triazol-1-ylmethyl)piperazine Chemical compound C1=NC=NN1CN(CC1)CCN1CN1C=NC=N1 WHFGLPOOBLVZRM-UHFFFAOYSA-N 0.000 description 3
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 3
- VKZRWSNIWNFCIQ-UHFFFAOYSA-N 2-[2-(1,2-dicarboxyethylamino)ethylamino]butanedioic acid Chemical compound OC(=O)CC(C(O)=O)NCCNC(C(O)=O)CC(O)=O VKZRWSNIWNFCIQ-UHFFFAOYSA-N 0.000 description 3
- CABMTIJINOIHOD-UHFFFAOYSA-N 2-[4-methyl-5-oxo-4-(propan-2-yl)-4,5-dihydro-1H-imidazol-2-yl]quinoline-3-carboxylic acid Chemical compound N1C(=O)C(C(C)C)(C)N=C1C1=NC2=CC=CC=C2C=C1C(O)=O CABMTIJINOIHOD-UHFFFAOYSA-N 0.000 description 3
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Images
Classifications
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- 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
- G03C7/42—Bleach-fixing or agents therefor ; Desilvering processes
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- 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
- G03C7/44—Regeneration; Replenishers
Definitions
- the present invention relates to a method for processing a silver halide color photographic light-sensitive material, and more specifically to a bleaching step that regenerates the overflow of a bleaching solution and recycles it.
- the processing of silver halide color photographic light-sensitive materials basically consists of a color-development step and a desilvering step, and the desilvering step is carried out in two steps, i.e., bleaching and fixing, or in one step, i.e., bleach-fixing, or in a step made up of a combination of these. Processing steps other than these include a washing step, a stabilizing step, a rinsing step, etc.
- the bleaching step developed silver that results from the reduction of a silver halide in the light-sensitive material in a developing bath with a developer, is oxidized with an oxidizing agent, called a bleaching agent, to a silver salt that can be fixed. At that time, the bleaching agent is reduced, in an amount equivalent to the silver that has been oxidized.
- the processing is carried out with a bleaching replenisher containing a fresh oxidizing agent be being added (replenished).
- the replenishment causes the bleaching solution to be discharged as a processing waste liquor, in an amount corresponding to the added amount of the replenisher.
- reduction of the amount of processing waste liquor in view of problems, including water contamination, etc. has become an important demand in the market.
- the latter regeneration of a bleaching solution is a method in which the overflow from a bleaching bath, which overflow will otherwise become waste liquor, is stored outside the bleaching solution tank, and bleaching solution components that have been reduced, for example, due to dilution with the carried-over solution from the preceding bath, consumption in the reaction, and the carryover to the succeeding bath by adhesion to the light-sensitive material, are supplied (replenished) to the stored overflow, so that it can be used as a replenisher again.
- a method for replenishing bleaching solution components a method is well known wherein, when the overflow is regenerated, out of the bleaching solution components, those that have been consumed, such as a bleaching agent and a rehalogenating agent in the bleaching solution, are added to the overflow from the bleaching bath.
- a bleaching agent among them in order to minimize the amount of the agent to be added freshly, a means is known wherein the bleaching agent whose bleaching capacity has been lost by the reaction of oxidizing developed silver is oxidized again, to make it regain its original bleaching capacity.
- one of such means is a technique wherein, by adding another oxidizing agent that is more powerful than the bleaching agent, the reduced bleaching agent is restored to a form capable of bleaching, so that the activity of the bleaching solution can be restored, the handling of the powerful oxidizing agent is inconvenient, and there is also a problem that the accumulation of the salt resulting from the addition of the agent hampers the bleaching speed.
- As another oxidation technique for restoring the activity of a bleaching agent there is a method wherein air is bubbled through the bleaching solution, to allow the oxygen in the air to oxidize the bleaching agent. This method is simple and is used widely in the market.
- This method causes less of an environmental pollution problem, and, as a bleaching agent that can be regenerated by a simple oxidation method, such as aeration, a ferric complex salt of ethylenediaminetetraacetic acid or 1,3-diaminopropanetetraacetic acid is used currently, in many cases.
- a simple oxidation method such as aeration
- a ferric complex salt of ethylenediaminetetraacetic acid or 1,3-diaminopropanetetraacetic acid is used currently, in many cases.
- the bleaching solution that uses the former has low oxidizing power, it is used in a high concentration or in combination with a bleaching accelerator, to secure bleaching speed.
- a problem common to both of them is lowering of the operability due to the bubbling during the aeration. That is, surfactants and polymer components that mainly ooze from the light-sensitive material accumulate in the bleaching solution, causing such a problem as that the long-period aeration at the regeneration brings about violent bubbling from the vessel, to pollute the working environment or to cause part of the solution to flow out, making it impossible to secure the desired amount of the regenerated bleaching solution.
- the bubbling is apt to increase, and therefore an operation of breaking the bubbles, such as interruption of the aeration, is needed.
- An object of the present invention is to provide a method for processing a silver halide color photographic light-sensitive material, in which method, when a regenerated bleaching solution is used, stain and fogging are suppressed, bubbling at the time of regeneration is suppressed, the efficiency of the regeneration operation is improved, and a bleaching solution can be regenerated and used without impairing the bleaching performance, with the load on the environment reduced.
- Fig. 1 shows a flow sheet of the method of the invention, which illustrates regenerating the overflow of a bleaching solution, to use it as a replenisher.
- the effect of preventing stain that contributes to a Dmin increase by controlling the pH of the washing bath after the bleaching is distinctive when the aminopolycarboxylic acid iron(III) complex salt represented by formula (I) for use in the present invention is used. It is unexpected from the situation of the conventional use of ethylenediaminetetraacetic acid and 1,3-diaminopropanetetraacetic acid, that the simple method wherein pH is adjusted has opened an effective way of solving the problems.
- the bleaching solution used in the present invention is characterized in that the ferric complex salt of the compound represented by formula (I) is regenerated, to be used in such a manner that the amount of a bleaching solution regenerating agent used, per square meter of the light-sensitive material to be processed, is smaller than the amount of the solution carried over from the color-developing bath, per that area.
- R 1 represents a hydrogen atom, an aliphatic hydrocarbon group, an aryl group, or a heterocyclic group
- L 1 and L 2 each represent an alkylene group
- M 1 and M 2 each represent a hydrogen atom or a cation.
- the number of carbon atoms hereinafter referred to means a number of carbon atoms, excluding that in a substituent moiety.
- Examples of the aliphatic hydrocarbon group represented by R 1 include a straight-chain, branched, or cyclic alkyl group having preferably 1 to 12, more preferably 1 to 10, and still more preferably 1 to 8 carbon atoms; an alkenyl group having preferably 2 to 12, more preferably 2 to 10, and still more preferably 2 to 7 carbon atoms; and an alkynyl group having preferably 2 to 12, more preferably 2 to 10, and still more preferably 2 to 7 carbon atoms, each of which may be substituted with a substituent.
- Examples of such a substituent include an aryl group having preferably 6 to 12, more preferably 6 to 10, and particularly preferably 6 to 8 carbon atoms (e.g. phenyl, p-methylphenyl); an alkoxy group having preferably 1 to 8, more preferably 1 to 6, and particularly preferably 1 to 4 carbon atoms (e.g. methoxy, ethoxy); an aryloxy group having preferably 6 to 12, more preferably 6 to 10, and particularly preferably 6 to 8 carbon atoms (e.g. phenyloxy); an acyl group having preferably 1 to 12, more preferably 2 to 10, and particularly preferably 2 to 8 carbon atoms (e.g.
- acetyl an alkoxycarbonyl group having preferably 2 to 12, more preferably 2 to 10, and particularly preferably 2 to 8 carbon atoms (e.g. methoxycarbonyl); an acyloxy group having preferably 1 to 12, more preferably 2 to 10, and particularly preferably 2 to 8 carbon atoms (e.g. acetoxy); an acylamino group having preferably 1 to 10, more preferably 2 to 6, and particularly preferably 2 to 4 carbon atoms (e.g. acetylamino); a sulfonylamino group having preferably 1 to 10, more preferably 1 to 6, and particularly preferably 1 to 4 carbon atoms (e.g.
- methanesulfonylamino a sulfamoyl group having preferably 0 to 10, more preferably 0 to 6, and particularly preferably 0 to 4 carbon atoms (e.g. sulfamoyl and methylsulfamoyl); a carbamoyl group having preferably 1 to 10, more preferably 1 to 6, and particularly preferably 1 to 4 carbon atoms (e.g. carbamoyl and methylcarbamoyl); an alkylthio group having preferably 1 to 8, more preferably 1 to 6, and particularly preferably 1 to 4 carbon atoms (e.g.
- a sulfonyl group having preferably 1 to 8, more preferably 1 to 6, and particularly preferably 1 to 4 carbon atoms e.g. methanesulfonyl
- a sulfinyl group having preferably 1 to 8, more preferably 1 to 6, and particularly preferably 1 to 4 carbon atoms e.g. methanesulfinyl
- a heterocyclic group e.g. imidazolyl, pyridyl.
- Preferred among the above-listed substituents for the aliphatic hydrocarbon groups represented by R 1 are an alkoxy group, a carboxyl group, a hydroxyl group, and a sulfo group, and more preferred are a carboxyl group and a hydroxyl group.
- Preferred among the aliphatic hydrocarbon groups represented by R 1 is an alkyl group, more preferably a chain alkyl group. Still more preferable examples thereof include methyl, ethyl, carboxymethyl, 1-carboxyethyl, 2-carboxyethyl, 1,2-dicarboxyethyl, 1-carboxy-2-hydroxyethyl, 2-carboxy-2-hydroxyethyl, 2-hydroxyethyl, 2-methoxyethyl, 2-sulfoethyl, 1-carboxypropyl, 1-carboxybutyl, 1,3-dicarboxypropyl, 1-carboxy-2-(4-imidazolyl)ethyl, 1-carboxy-2-phenylethyl, 1-carboxy-3-methylthiopropyl, 2-carbamoyl-1-carboxyethyl, and 4-imidazolylmethyl; and the particularly preferred are methyl, carboxymethyl, 1-carboxyethyl, 2-car
- aryl groups represented by R 1 is an aryl group composed of a single ring or twin rings, each having 6 to 20 carbon atoms (e.g. phenyl and naphthyl); more preferred is an aryl group having 6 to 15 carbon atoms; and still more preferred is an aryl group having 6 to 10 carbon atoms.
- the aryl group represented by R 1 may have a substituent, examples of which include an alkyl group having preferably 1 to 8, more preferably 1 to 6, and particularly preferably 1 to 4 carbon atoms (e.g. methyl and ethyl); an alkenyl group having preferably 2 to 8, more preferably 2 to 6, and particularly preferably 2 to 4 carbon atoms (e.g. vinyl and allyl); and an alkynyl group having preferably 2 to 8, more preferably 2 to 6, and particularly preferably 2 to 4 carbon atoms (e.g. propargyl), in addition to the above-listed groups as the substituents for the aliphatic hydrocarbon group represented by R 1 .
- a substituent examples of which include an alkyl group having preferably 1 to 8, more preferably 1 to 6, and particularly preferably 1 to 4 carbon atoms (e.g. methyl and ethyl); an alkenyl group having preferably 2 to 8, more preferably 2 to 6, and particularly preferably 2 to 4 carbon atoms (e
- Preferred among the substituents for the aryl group represented by R 1 are an alkyl group, an alkoxy group, a hydroxyl group, and a sulfo group; and more preferred are an alkyl group, a carboxyl group, and a hydroxyl group.
- aryl group represented by R 1 examples include 2-carboxyphenyl and 2-carboxymethoxyphenyl.
- the heterocyclic group represented by R 1 is a residue of a 3- to 10-membered saturated or unsaturated heterocyclic compound containing at least one of N, O, and S atoms, which may be a single ring or a condensed ring with another ring.
- heterocyclic groups is a 5- or 6-membered aromatic heterocyclic group, with a more preferred example being a 5- or 6-membered nitrogen atom-containing aromatic heterocyclic group. Still more preferred is a 5- or 6-membered aromatic heterocyclic group containing one or two nitrogen atoms.
- heterocyclic group examples include pyrrolidinyl, piperidyl, piperazinyl, imidazolyl, pyrazolyl, pyridyl, and quinolyl.
- Preferred among these groups are an imidazolyl group and a pyridyl group.
- the heterocyclic group represented by R 1 may have a substituent, examples of which include an alkyl group having preferably 1 to 8, more preferably 1 to 6, and particularly preferably 1 to 4 carbon atoms (e.g. methyl and ethyl); an alkenyl group having preferably 2 to 8, more preferably 2 to 6, and particularly preferably 2 to 4 carbon atoms (e.g. vinyl and allyl); and an alkynyl group having preferably 2 to 8, more preferably 2 to 6, and particularly preferably 2 to 4 carbon atoms (e.g. propargyl), in addition to the above-listed groups as the substituents for the aliphatic hydrocarbon group represented by R 1 .
- a substituent examples of which include an alkyl group having preferably 1 to 8, more preferably 1 to 6, and particularly preferably 1 to 4 carbon atoms (e.g. methyl and ethyl); an alkenyl group having preferably 2 to 8, more preferably 2 to 6, and particularly preferably 2 to 4 carbon atoms (e
- Preferred among the substituents for the heterocyclic group represented by R 1 are an alkyl group, an alkoxy group, a hydroxyl group, and a sulfo group; and more preferred are an alkyl group, a carboxyl group, and a hydroxyl group.
- R 1 is preferably a hydrogen atom, or an alkyl group having 1 to 8 carbon atoms, and more preferred is a hydrogen atom, a methyl group, an ethyl group, a 1-carboxyethyl group, a 2-carboxyethyl group, a hydroxyethyl group, or a 2-carboxy-2-hydroxyethyl group.
- a hydrogen atom is especially preferred.
- the alkylene groups represented by L 1 and L 2 are the same or different, and they may be straight chain, branched chain, or cyclic groups. Further, they may have a substituent, examples of which include an alkenyl group having preferably 2 to 8, more preferably 2 to 6, and particularly preferably 2 to 4 carbon atoms (e.g. vinyl and allyl); and an alkynyl group having preferably 2 to 8, more preferably 2 to 6, and particularly preferably 2 to 4 carbon atoms (e.g. propargyl), in addition to the above-listed groups as the substituent for the aliphatic hydrocarbon group represented by R 1 .
- Preferred among the substituents for the alkylene groups represented by L 1 and L 2 are an aryl group, an alkoxy group, a hydroxy group, a carboxyl group, and a sulfo group; and more preferred are an aryl group, a carboxyl group, and a hydroxyl group.
- Preferred alkylene groups represented by L 1 and L 2 are groups whose alkylene moieties have 1 to 6 carbon atoms, and more preferably 1 to 4 carbon atoms. Still more preferred alkylene groups are substituted or unsubstituted methylene and ethylene groups.
- alkylene group examples include methylene, ethylene, trimethylene, methylmethylene, ethylmethylene, n-propylmethylene, n-butylmethylene, 1,2-cyclohexylene, 1-carboxymethylene, carboxymethylmethylene, carboxyethylmethylene, hydroxymethylmethylene, 2-hydroxyethylmethylene, carbamoylmethylmethylene, phenylmethylene, benzylmethylene, 4-imidazolylmethylmethylene, and 2-methylthioethylmethylene; and more preferred are methylene, ethylene, methylmethylene, ethylmethylene, n-propylmethylene, n-butylmethylene, 1-carboxymethylene, carboxymethylmethylene, carboxyethylmethylene, hydroxymethylmethylene, benzylmethylene, 4-imidazolylmethylmethylene, and 2-methylthioethylmethylene; and still more preferred are methylene, ethylene, trimethylene, methyl
- the cation represented by M 1 or M 2 is an organic or inorganic cation, examples of which include an alkali metal ion (e.g. Li + , Na + , K + , Cs + ), an alkali earth metal ion (e.g. Mg 2+ , Ca 2+ ), an ammonium ion (e.g. ammonium, trimethylammonium, triethylammonium, tetramethylammonium, tetraethylammonium, tetrabutylammonium, 1,2-ethanediammonium), a pyridinium ion, an imidazolium ion, and a phosphonium ion (e.g. tetrabutylphosphonium).
- Preferred examples of M 1 and M 2 are an alkali metal ion and an ammonium ion, and more preferred are Na + , K + , and NH 4 + .
- Preferred among the compounds represented by formula (I), are those represented by the following formula (I-a): wherein L 1 and M 1 each have the same meanings as those in formula (I), and therefore their preferred ones are also same; M a1 and M a2 each have the same meanings as M 2 in formula (I).
- Preferred among the compounds represented by formula (I-a), are those in which L 1 is a substituted or unsubstituted methylene or ethylene group, and M 1 , M a1 , and M a2 are any one of a hydrogen atom, an alkali metal, and an ammonium, respectively. More preferred compounds are ones in which L 1 is a substituted or unsubstituted methylene group, and M 1 , M a1 , and M a2 are any one of a hydrogen atom, an alkali metal, and an ammonium, respectively.
- Particularly preferred compounds are ones in which L 1 is a substituted or unsubstituted methylene group having 1 to 10 total carbon atoms including its substituent, and M 1 , M a1 , M a2 are any one of a hydrogen atom, Na + , K + , and NH 4 + , respectively.
- the compound represented by formula (I) has asymmetric carbon atoms in the molecule, preferably at least one asymmetric carbon atom is in an L-form.
- those compounds wherein L is annexed are ones wherein the asymmetric carbon section of the annexed part is in an L-form, and those wherein L is not annexed are mixtures of a D-form and a L-form.
- the above-listed compounds may be ones in which a hydrogen atom of the carboxyl group is substituted with a cation, respectively.
- the cation has the same meanings as defined for those represented by M 1 and M 2 in formula (I).
- the compound represented by formula (I) for use in the present invention can be prepared according to the methods described in, for example, Journal of Inorganic and Nuclear Chemistry , Vol. 35, p. 523 (1973), Swiss patent No. 561504, DE-A-3912551(A1), DE-A-3939755(A1), DE-A-3939756(A1), JP-A-5-265159 ("JP-A” means unexamined published Japanese patent application), JP-A-6-59422 (methods for preparing L-forms of exemplified compounds I-42, I-43, I-46, I-52, and I-53 are described in the synthesis examples 1, 2, 3, 4 and 6), JP-A-6-95319 (methods for preparing L forms of exemplified compounds I-8, I-11, I-37, I-38, and I-40 are described in the synthesis examples 2 to 6), JP-A-6-161054, and JP-A-6-161065.
- the replenisher is one that is added to each of the processing tanks, where processing is carried out, in conformity with the processed amount of the light-sensitive material at the time of the development processing, to carry out the development processing continuously and stably.
- the components thereof are those that supplement exhausted components and consumed components.
- the bleaching solution replenisher is prepared by adding a regenerating agent to the overflow. That is, the bleaching-solution replenisher comprises components required for the reuse of the overflow, which specifically include a bleaching agent, an organic acid, a pH adjustor, a rehalogenating agent, etc.
- the bleaching regenerating agent solution constituting the present invention is added to the overflow from the bleaching bath for use in the present invention, to prepare the bleaching replenisher.
- the bleaching-regenerating-agent solution basically comprises components contained in the bleaching solution described in detail later.
- the bleaching-regenerating-agent solution can contain, a bleaching agent and an organic acid, as well as a rehalogenating agent, for example, a bromide, such as potassium bromide, sodium bromide, and ammonium bromide, or a chloride, such as potassium chloride, sodium chloride, and ammonium chloride.
- a rehalogenating agent for example, a bromide, such as potassium bromide, sodium bromide, and ammonium bromide, or a chloride, such as potassium chloride, sodium chloride, and ammonium chloride.
- a plurality of rehalogenating agents can be used in combination.
- the concentration of the rehalogenating agent is generally 0.1 to 2 mol and preferably 0.2 to 1.5 mol, per liter of the bleaching solution.
- a nitrate such as sodium nitrate and ammonium nitrate, boric acid, borax, sodium metaborate, acetic acid, sodium acetate, sodium carbonate, potassium carbonate, phosphorous acid, phosphoric acid, and such salts as sodium phosphate can be added.
- a bleaching accelerator can be used in the bleaching-regenerating-agent solution for use in the present invention.
- bleaching accelerator for example, can be mentioned various mercapto compounds described, for example, in US-A-3 893 858, GB-A-1 138 842, JP-A-53-141623, JP-A-53-95631, and JP-A-54-52534, disulfide compounds described in JP-A-53-95630, thiourea derivatives described in JP-B-45-8506 ("JP-B" means examined Japanese patent publication) and JP-B-49-42349, isothiourea derivatives described in JP-A-53-94927, thiazolidine derivatives described in JP-B-53-9854, thioamide compounds described in JP-A-42349, and dithiocarbamates described in JP-A-55-26506.
- the pH of the bleaching-regenerating-agent solution that is used in the present invention is generally in the range of 2.8 to 4.0, preferably 3.0 or higher but 4.0 or lower, and particularly preferably 3.1 to 3.9.
- the above mentioned dicarboxylic acids as well as organic acids, inorganic acids, and alkalis can be used, and it is preferable to adjust the amount of acetic acid, nitric acid, sodium hydroxide, potassium hydroxide, ammonia, or the above mentioned dicarboxylic acids.
- the regenerating agent is introduced into a separately provided storage tank for the overflow, where the solution thereof is prepared, and then it is transferred to a replenishment tank.
- the solution carried into the bleaching bath from the color-developing bath varies depending on the processor and the setting conditions, it is approximately constant, generally in the range of 30 to 100 ml/m 2 , and preferably 40 to 90 ml/m 2 .
- the bleaching replenisher when the bleaching replenisher is prepared by adding the bleaching agent to the overflow from the bleaching bath that results from the replenishment, it is characterized in that the amount of the regenerating agent is made smaller than the amount of the solution carried into the bleaching bath from the above color-development bath. That is, it is characterized by the following relationship.
- the amount of the bleaching replenisher required in the processing of a square meter of the light-sensitive material to be processed is equal to the amount of the overflow from the bleaching bath that results from the processing of a square meter of the light-sensitive material to be processed
- a ferric (iron (III)) complex salt of a compound represented by formula (I) may be added in the form of an isolated compound.
- the compound of formula (I) and a ferric salt e.g. ferric nitrate, ferric chloride
- ferric salt e.g. ferric nitrate, ferric chloride
- the compound of formula (I) for use in the present invention may be used singly or in a combination of two or more kinds thereof.
- the compound of formula (I) may be used somewhat in excess of the amount necessary to form a complex salt of ferric ion (e.g. 0.5, 1, or 2 times the molar amount per the ferric ion).
- the excess amount is generally regulated to the range of 0.01 to 15 mol%.
- the amount of 1,3-diaminopropanetetraacetic acid and/or ethylenediaminetetraacetic acid in the aminopolycarboxylic acid(s) of the iron(III) complex salt of the aminopolycarboxylic acid compound in the bleaching solution used in the present invention is preferably 1/2 or less, but 0 or more, and more preferably 1/3 or less, but 0 or more, in terms of molar fraction.
- a ferric complex salt of an organic acid contained in a processing solution having bleaching capacity for use in the present invention may be used in the form of an alkali metal salt or an ammonium salt.
- Example alkali metal salts are a lithium salt, a sodium salt, and a potassium salt.
- example ammonium salts are an ammonium salt and a tetraethylammonium salt.
- the concentration of an ammonium ion in a processing solution having bleaching capacity is preferably 0 to 0.4 mol/l, and especially preferably 0 to 0.2 mol/l.
- the above iron complex salts of organic acids can be used singly or in combination of two or more.
- the bleaching solution contains a dicarboxylic acid, a hydrocarboxylic acid, or a sulfocarboxylic acid.
- These acid compounds refer to saturated carboxylic acids, unsaturated carboxylic acids, and aromatic carboxylic acids, or their alkali metal salts and ammonium salts, that have, in the molecule, a carboxylic group and further one carboxylic group, a hydroxyl group, or a sulfo group.
- a dicarboxylic acid, a hydroxycarboxylic acid, or a sulfocarboxylic acid represented by the below-shown formula (D) and their salts are preferable: X-L-COOH wherein L represents a saturated or unsaturated aliphatic group having 1 to 4 carbon atoms, and X represents a carboxyl group, a hydroxy group, or a 1-sulfocarboxymethyl group.
- a preferable amount of this acid to be added is generally in the range of 0.1 to 2.0 mol and more preferably 0.3 to 1.5 mol, per liter of the bleaching solution.
- these acids are mentioned below, but the present invention is not limited to them: oxalic acid, malonic acid, succinic acid, glutaric acid, adipic acid, maleic acid, fumaric acid, malic acid, tartaric acid, phthalic acid, glycolic acid, diglycolic acid, aspartic acid, glutamic acid, sulfosuccinic acid, and the like.
- malonic acid, succinic acid, glycolic acid, glutaric acid, and maleic acid are particularly preferable and preferably two or more of them are used in combination.
- a combination of succinic acid with maleic acid or a combination of glycolic acid with succinic acid or malonic acid is most preferable.
- the bleaching solution constituting the present invention can contain, in addition to the bleaching agent and the above compounds, a rehalogenating agent, for example, a bromide, such as potassium bromide, sodium bromide, and ammonium bromide, and a chloride, such as potassium chloride, sodium chloride, and ammonium chloride. Two or more of the rehalogenating agents may be used in combination.
- the concentration of the rehalogenating agent is generally 0.1 to 2 mol and preferably 0.2 to 1.5 mol, per liter of the bleaching solution.
- a nitrate such as sodium nitrate and ammonium nitrate, boric acid, borax, sodium metaborate, acetic acid, sodium acetate, sodium carbonate, potassium carbonate, phosphorous acid, phosphoric acid, and such salts as sodium phosphate can be added.
- a bleaching accelerator can be used in the bleaching solution for use in the present invention.
- the bleaching accelerator can be used, for example, various mercapto compounds described, for example, in US-A-3 893 858, GB-A-1 138 842, JP-A-53-141623, JP-A-53-95631, and JP-A-54-52534, disulfide compounds described in JP-A-53-95630, thiourea derivatives described in JP-B-45-8506 and JP-B-49-42349, isothiourea derivatives described in JP-A-53-94927, thiazolidine derivatives described in JP-B-53-9854, thioamide compounds described in JP-A-42349, and dithiocarbamates described in JP-A-55-26506.
- the bleaching solution for use in the present invention contains at least one of 1,2-benzoisothiazolin-3-one or its derivatives. Specific examples of these compounds are given below, which do not limit the present invention:
- 1,2-benzoisothiazolin-3-one 2-methyl-1,2-benzoisothiazolin-3-one, 2-ethyl-1,2-benzoisothiazolin-3-one, 2-(n-propyl)-1,2-benzoisothiazolin-3-one, 2-(n-butyl)-1,2-benzoisothiazolin-3-one, 2-(sec-butyl)-1,2-benzoisothiasolin-3-one, 2-(t-butyl)-1,2-benzoisothiazolin-3-one, 2-methoxy-1,2-benzoisothiazolin-3-one, 2-ethoxy-1,2-benzoisothiazolin-3-one, 2-(n-propyloxy)-1,2-benzoisothiazolin-3-one, 2-(n-butyloxy)1,2-benzoisothiazolin-3-one, 5-chloro-1,2-benzoisothiazolin-3-one, 5-methyl-1,2-benzois
- a preferable amount of these compounds to be added is 0.001 to 1 g, more preferably 0.01 to 0.5 g, and particularly preferably 0.02 to 0.2 g, per liter of the bleaching solution.
- These compounds may be added in the form of salts, and they may be added as a combination of two or more.
- the bleaching solution for use in the present invention preferably contains various antibacteria agents and mildewproofing agents.
- These antibacteria agents and mildewproofing agents are preferably at least one of benzoimidazole compounds, alkylguanidine compounds, succinic acid imide compounds, sulfimide compounds, isothiazolone compounds, hydroxybenzoate ester compounds, phenoxyalcohol compounds, and quaternary ammonium salts described in JP-A-8-339063, or aminoglycocides selected from the group consisting of genatamicins, amikacin, tobramycin, dibekacin, arbekacin, micronomicin, isepamicin, sisomicin, netilmicin, and astromicin.
- benzoisothiazolone compounds are more preferable and particularly 1,2-benzoisothiazolin-3-one is preferable. Further, two or more of these antibacteria agents and mildewproofing agents can be used in combination in various ratios.
- the bleaching solution for use in the present invention preferably contains derivatives of picolinic acid.
- the picolinic acid derivatives include, in addition to picolinic acid, 2,6-pyridinedicarboxylic acid, 4-chloro-2,6-pyridinedicarboxylic acid, 4-hydroxy-2,6-pyridinedicarboxylic acid, 4-methoxy-2,6-pyridinedicarboxylic acid, 2,3-pyridinedicarboxylic acid, 2,4-pyridinedicarboxylic acid, and 2,5-pyridinedicarboxylic acid, and those described in JP-A-8-339063.
- picolinic acid 2,6-pyridinedicarboxylic acid, and 4-chloro-2,6-pyridinedicarboxylic acid are preferable, with particular preference given to 2,6-pyridinedicarboxylic acid.
- the amount of these compounds to be added is generallly suitably 0.005 to 3.0 mol/liter, preferably 0.01 to 2.0 mol/liter, and particularly preferably 0.05 to 1.50 mol/liter.
- a sulfinic acid compound represented by the following formula (S) is used: R-(SO 2 M) n wherein R represents an alkyl group, an alkenyl group, an aralkyl group, a cycloalkyl group, an aryl group, or a heterocyclic group, M represents a cation, and n is 1 or 2.
- R represents a substituted or unsubstituted alkyl group (e.g. methyl, ethyl, n-propyl, hydroxyethyl, sulfoethyl, carboxyethyl, and methoxyethyl), a substituted or unsubstituted alkenyl group (e.g. allyl and butenyl), a substituted or unsubstituted aralkyl group (e.g. benzyl, phenetyl, 4-carboxyphenylmethyl, and 3-sulfophenylmethyl), a substituted or unsubstituted cycloalkyl group (e.g.
- cyclohexyl a substituted or unsubstituted aryl group (e.g. phenyl, 4-methylphenyl, naphthyl, 3-carboxyphenyl, 4-methoxyphenyl, 3-sulfophenyl, 4-carboxymethoxyphenyl, 3-carboxymethoxyphenyl, 4-carboxyethoxyphenyl, 4-sulfoethoxyphenyl, 4-carboxymethylphenyl, and 4-(N-carboxymethyl-N-methyl)phenyl), or a substituted or unsubstituted heterocyclic group (e.g. pyridyl, furyl, thienyl, pyrazolyl, and indolyl).
- aryl group e.g. phenyl, 4-methylphenyl, naphthyl, 3-carboxyphenyl, 4-methoxyphenyl, 3-sulfophenyl, 4-carboxymethoxyphenyl
- M represents a cation, for example, a hydrogen atom, an alkali metal, an alkali earth metal, a nitrogen-containing organic base, or ammonium group.
- the alkali metal includes Na, K, Li, and the like; and the alkali earth metal includes Ca, Ba, and the like; and the nitrogen-containing organic base includes usual amines capable of forming bases with sulfinic acid; and the ammonium group includes an unsubstituted ammonium group, a tetramethylammonium group, and the like.
- R when the group represented by R has a substituent, examples thereof are a nitro group, a halogen atom (e.g. chlorine and bromine), a cyano group, an alkyl group (e.g. methyl, ethyl, propyl, carboxymethyl, carboxyethyl, carboxypropyl, sulfoethyl, sulfopropyl, and dimethylaminoethyl), an aryl group (e.g. phenyl, naphthyl, carboxyphenyl, and sulfophenyl), an alkenyl group (e.g. allyl and butenyl), an aralkyl group (e.g.
- benzyl and phenetyl a sulfonyl group (e.g. methanesulfonyl and p-toluenesulfonyl), an acyl group (e.g. acetyl and benzoyl), a carbamoyl group (e.g. unsubstituted carbamoyl and dimethylcarbamoyl), a sulfamoyl group (e.g. unsubstituted sulfamoyl, methylsulfamoyl, and dimethylsulfamoyl), a carbonamido group (e.g.
- acetamido and benzamido a sulfonamido group (e.g. methanesulfonamido and benzenesulfonamido), an acyloxy group (e.g. acetyloxy and benzoyloxy), a sulfonyloxy group (e.g. methanesulfonyloxy), a ureido group (e.g. unsubstituted ureido), a thioureido group (e.g.
- unsubstituted thioureido and methylthioureido a carboxylic acid or its salt, a sulfonic acid or its salt, a hydroxy group, an alkoxy group (e.g. methoxy, ethoxy, carboxyethoxy, carboxymethoxy, sulfoethoxy, and sulfopropyloxy), an alkylthio group (e.g. methylthio, carboxymethylthio, and sulfoethylthio), and an amino group (e.g. unsubstituted amino, dimethylamino, and N-carboxyethyl-N-methylamino).
- an alkoxy group e.g. methoxy, ethoxy, carboxyethoxy, carboxymethoxy, sulfoethoxy, and sulfopropyloxy
- an alkylthio group e.g. methylthio, carboxymethylthio
- S-2, S-4, S-7, and S-11 are preferable, with particular preference given to S-7.
- a suitable amount of these compounds to be used is generally 0.005 to 0.1 mol, preferably 0.01 to 0.08 mol, and more preferably 0.015 to 0.05 mol, per liter of the bleaching solution. Two or more of them may be used in combination.
- a surfactant selected from the group consisting of those represented by the following formulae (II) and (III): RO(CH 2 CH 2 O) m [CH 2 CH(OH)CH 2 O] n X wherein R represents a straight-chain or branched and optionally substituted alkyl group having 8 to 25 carbon atoms or in which R 1 represents a straight-chain or branched alkyl group having 6 to 20 carbon atoms, R 2 represents a hydrogen atom or a straight-chain or branched alkyl group having 1 to 20 carbon atoms, l is an integer of 0 to 4; and wherein when n is 0, m is 40 to 200, when n is 5 to 9, m is 10 to 100, when n is 10 or more, m is 0 to 100, n being 0 or an integer of 5 to 50, and X represents a hydrogen atom or SO 3 M in which M represents a hydrogen atom or an
- R 1 represents an optionally substituted alkyl group, alkenyl group, or alkoxyalkyl group
- R 2 represents a hydrogen atom, an alkyl group, a hydroxyalkyl group, or an alkoxy group
- R 3 and R 4 independently represent a hydrogen atom, a hydroxyl group, an optionally substituted alkyl group, or CO 2 M 1
- M and M 1 each represent a hydrogen atom or an alkali metal
- n is 0 or 1.
- surfactants have an effect of dispersing and solubilizing the above-described tar, to prevent the tar from adhering to the light-sensitive material to be processed, but it is an unexpected matter that surfactants have, in addition to the above effect, an effect of preventing fogging, which is one object of the present invention.
- surfactants that have shown a particularly high effect, that is, the compounds represented by formula (II) or (III), are described.
- R when R is a straight-chain or branched and optionally substituted alkyl group having 8 to 25 carbon atoms, preferably R has 9 to 18 carbon atoms and particularly preferably 10 to 16 carbon atoms.
- R 2 represents a straight-chain or branched alkyl group having 1 to 20 carbon atoms, and particularly preferably a methyl group, an ethyl group, an n- or i-propyl group, an n-, i-, or t-butyl group, a pentyl group, an n- or t-octyl group, or a nonyl group.
- n is an integer of 40 to 200, preferably 50 to 150, and more preferably 80 to 130.
- n is from 5 to 9
- m is an integer of 10 to 100, preferably 20 to 80, and more preferably 30 to 70.
- n is 10 or more
- m is an integer of 0 to 100, preferably 5 to 50, and more preferably 10 to 40.
- n is 0 or an integer of 5 to 50, preferably 0 or an integer of 5 to 30, and particularly preferably 0 or an integer of 10 to 20.
- X represents a hydrogen atom or SO 3 M, preferably a hydrogen atom
- M represents a hydrogen atom or an alkali metal, and preferably sodium.
- R 1 represents an optionally substituted alkyl group, alkenyl group, or alkoxyalkyl group having 3 to 30 carbon atoms, preferably 5 to 18 carbon atoms, and more preferably 8 to 16 carbon atoms.
- Preferable substituents thereof are, for example, an alkyl group, an alkenyl group, an alkoxyalkyl group, a carboxyalkyl group, a sulfoalkyl group, a dicarboxyalkyl group, and a sulfocaboxyalkyl group, and particularly preferable examples include a dicarboxymethyl group and a sulfocarboxymethyl group.
- R 2 represents a hydrogen atom, an alkyl group, a hydroxyalkyl group, an alkoxy group, or an alkoxyalkyl group
- R 2 and R 4 independently represent a hydrogen atom, a hydroxyl group, an optionally substituted alkyl group, such as a carboxyalkyl group, or CO 2 M 1
- M and M 1 each represent a hydrogen atom or an alkali metal
- n is 0 or 1.
- a lower carboxyalkyl group such as a carboxymethyl group and a carboxyethyl group
- a lower alkyl group such as a methyl group, an ethyl group, and a propyl group, are preferable.
- the amount of the surfactants of formula (II) or (III) to be added is generally 0.02 to 5 g, preferably 0.1 to 3 g, and more preferably 0.2 to 2 g, per liter of the bleaching solution.
- a combination of the surfactants of formulae (II) and (III) can increase the effect more, and in that case the amount of each of them to be added is generally 0.01 to 3 g, preferably 0.04 to 2 g, and more preferably 0.1 to 1 g, per liter of the bleaching solution, with the total amount being generally 0.02 to 5 g, preferably 0.1 to 3 g, and more preferably 0.2 to 2 g, per liter of the bleaching solution.
- Each of the concentrations of components in a mother liquid can be kept constant by the above-described replenishing solution.
- the amount of the bleaching agent to be used is suitably generally 0.005 to 3.0 mol/l, preferably 0.02 to 2.0 mol/l, and particularly preferably 0.05 to 1.50 mol/l.
- the pH of the solution is suitably in the range of generally 2.9 to 7.5, preferably 3.1 to 6.5, and particularly preferably 3.3 to 5.5.
- an organic or inorganic acid or alkali can be used, and it is preferable to adjust the amount of acetic acid, nitric acid, sodium hydroxide, potassium hydroxide, ammonia, or the above-mentioned dicarboxylic acids.
- a suitable processing time is in the range of generally 40 sec to 10 min, preferably 1 min 30 sec to 8 min, and particularly preferably 2 to 7 min.
- a suitable processing time is in the range of generally 10 sec to 3 min, preferably 15 sec to 2 min, and more preferably 20 sec to 1 min 45 sec.
- the pH value of the bleaching replenisher is set to be lower, by about 0.1 to 1.0, than that of the bleaching solution.
- the replenishment is also preferably carried out by using a replenisher prepared by regenerating the overflow.
- the amount of the overflow from the bleaching bath corresponds substantially to the replenishment rate to the bleaching bath, and it is, in the case of color photographing materials, generally 100 to 2,000 ml, preferably 150 to 1,500 ml, and more preferably 300 to 1,000 ml, per square meter of the light-sensitive material to be processed, and in the case of print materials, generally 20 to 900 ml, preferably 25 to 500 ml, and more preferably 30 to 200 ml.
- the term "overflow” means the bleaching solution taken out from the bleaching bath for the renewal involved in the replenishment of the solution described above, and it does not necessarily mean one that overflows in its phenomenon.
- the proportion of the overflow that is reused is generally 0.1 to 1, preferably 0.2 to 1, and more preferably 0.5 to 1, assuming the entirety to be 1.
- a bleaching-solution-regenerating-agent solution is added to the overflow, to make a bleaching replenisher, and when it is used as a replenisher, the effect of the present invention is remarkable.
- replenishment corresponding to the processed amount of the light-sensitive material is made for the processing tank, and an overflow corresponding to the replenishment rate is discharged from the bleaching tank.
- the overflow may be, for example, pumped out, the overflow can be taken out simply by forming a notch or hole in an upper part of the bleaching tank.
- the overflow is temporary stored in a tank outside the bleaching tank, and when a certain amount is stored, it is processed batchwise.
- the bleaching solution developed silver that results from the reduction of the silver halide in the light-sensitive material with the developing agent in the developing bath, is oxidized with an oxidizing agent, called a bleaching agent, to silver ions. At that time, the bleaching agent is reduced in an amount equivalent to the oxidized silver. At the time of regeneration, the reduced bleaching agent is oxidized with oxygen in the air introduced into the bleaching solution by aeration, to turn (restore) the reduced bleaching agent into the original bleaching agent. This aeration step can be carried out in the processing tank directly.
- a means known in the art can be used, and, for example, blowing of air into a liquid having a bleaching capacity, or absorption of air by using an ejector, can be used.
- air When air is blown, preferably air is discharged into the liquid through aeration tubes having fine pores.
- the regeneration operation of the overflow of the bleaching solution can be carried out by adding the above-described bleaching-solution-regenerating agent to the overflow that has been subjected to the above aeration, and the resulting solution can be used as a replenisher.
- the bleaching-solution-regenerating agent is made up basically of the same components as the replenisher and the working solution, and the concentration thereof is generally higher than that of the replenisher.
- the addition of the bleaching-solution-regenerating agent makes the overflow that has been subjected to aeration reusable as a replenisher.
- the amount of the bleaching-solution-regenerating-agent solution is preferably 0.03 to 0.2 times, and more preferably 0.04 to 0.15 times, the amount of the overflow of the bleaching solution.
- the amount of the bleaching-solution-regenerating-agent solution is preferably 0.03 to 0.1 times, and more preferably 0.04 to 0.09 times, the amount of the overflow of the bleaching solution.
- the amount of the bleaching-solution-regenerating-agent solution is preferably 0.05 to 0.2 times, and more preferably 0.07 to 0.15 times, the amount of the overflow of the bleaching solution.
- the amount of the solution is decreased due to the concentration or the like, or the components of the developing solution are increased relatively, which likely leads to a risk of crystallization and precipitation.
- the amount is too large, the solution is increased at the time of the regeneration, and the merit that the regeneration of the overflow reduces the waste liquor is lost.
- the amount of the regenerating agent used, per square meter of the light-sensitive material to be processed becomes smaller than the amount of the solution carried over from the color-developing bath, per that area. That is, the amount of the regenerating agent used, per square meter of the light-sensitive material to be processed, is preferably 0.96 times or less (the volume ratio B/A, wherein A and B are as defined above), more preferably 0.92 times or less, and particularly preferably 0.88 times or less, the amount of the solution carried over from the color-developing bath, per that area.
- the amount of the regenerating agent used, per square meter of the light-sensitive material to be processed is 0.60 times or more, the amount of the solution carried over from the color-developing bath, per that area.
- the lower limit of the amount of the solution of the bleaching-solution-regenerating agent is preferably 18 ml or more, and more preferably 24 ml or more, per square meter of the light-sensitive material to be processed.
- the ammonium salts in the formulation accumulate in rivers, lakes, and ponds, it is known that the water is made eutrophic, to affect the environment.
- the ammonium salts can be replaced with alkali metal salts.
- the sodium salt and potassium salt of an organic acid ferric complex salt potassium bromide, sodium bromide, potassium nitrate, sodium nitrate, and the like are preferably used.
- ammonia water used in adjusting the pH is changed to potassium hydroxide or sodium hydroxide.
- ammonium salts are used in a liquid having a bleaching capacity.
- the great reason why ammonium salts are used in a liquid having a bleaching capacity is to increase the bleaching speed.
- salts other than ammonium salts can be used without any problems.
- a processing step of washing is provided after the bleaching step.
- the pH of the processing step of washing is preferably 3.5 to 8.0, more preferably 3.8 to 7.0, and further more preferably 4.0 to 6.0.
- the iron complex diffused in the light-sensitive layers of the light-sensitive material to be processed during the bleaching is washed out from the light-sensitive layers by this washing after the bleaching. At that time, the iron complex must be removed from the gelatin films forming the light-sensitive layers, with the complex structure kept stably. However, if the iron complex is low in stability, the complex dissociates in the films, and the remained iron causes stain.
- the iron(III) complex of the monoamine compound represented by formula (I) for use in the present invention described above is less stable, that is, small in the stability constant of iron complex, in comparison with iron(III) complexes of ethylenediaminetetraacetic acid or 1,3-diaminopropanetetraacetic acid, which are hitherto widely used diamine compounds.
- the stability constant and magnitude thereof mentioned herein is described in detail in "Nyumon Chelate Kagaku", written by Kagehei Ueno (Nanko-do), page 122.
- the present inventors have found that the above problems can be avoided only by controlling the pH of the washing bath after the bleaching step, as described above.
- the effect obtained by controlling the pH is also effective in preventing the precipitation of iron hydroxide, which results from the dissociation of the iron complex in the washing bath, and which is unpreferable in view of the processing operation.
- the control of the pH of the washing water may be carried out in any way known hitherto, and the method of controlling the pH of the washing water is not limited in the present invention.
- the method of controlling the pH of the washing water is not limited in the present invention.
- there are a method wherein an acid or an alkali is used to control the pH a method wherein an ion exchanger is used, and a method wherein an acid or an alkali produced by electrolysis is used.
- the pH is controlled with an inorganic acid, such as sulfuric acid and nitric acid;, an organic acid, such as acetic acid and citric acid; an alkali metal salt, an alkali earth metal salt, or ammonia.
- This pH control is preferably carried out by automatic control using a pH-stat or the like.
- the washing step prior to the stabilization can be omitted.
- the final stabilizing bath can also be omitted.
- the light-sensitive material that can be applied to the present invention may be any color light-sensitive materials, with preference given to color negative films, color reversal films, or color print papers.
- a color reversal light-sensitive material is processed, prior to the above steps, black-and-white development, reversal exposure or processing using a reversal bath, and, if necessary, a washing step are carried out.
- solutions containing, as a preservative, a substituted hydroxylamine, as described in JP-A-3-158849 or JP-A-3-174152 are preferable, and in particular, solutions containing a hydroxylamine having a sulfoalkyl group as a substitutent are preferable.
- solutions containing, as a chelating agent, diethylenetriaminepentaacetic acid, 1-hydroxyethylidene-1,1-diphosphonic acid, or 4,5-dihydroxybenzene-1,3-disulfonic acid are preferable.
- the replenisher of the color developer is preferably one whose bromide ion concentration is lowered to 0.004 mol/liter or less and particularly preferably 0.002 mol/liter or less, in view of the reduction of the replenishment rate.
- the color developer can be mentioned color developers and color development replenishers of Process CN-16X, CN-16Q, and CN-16FA (trade name) manufactured by Fuji Photo Film Co., Ltd., a color developer and a color-development replenisher of Process CR-56P (trade name) manufactured by Fuji Photo Film Co., Ltd.
- the color developer is preferably replenished with a color development replenisher.
- the color development replenisher contains the compounds contained in the color developer.
- the role of the color development replenisher is to replenish the color developer with compounds that have been decreased due to the processing of the light-sensitive material, and due to their deterioration with time in the automatic processor, and, in contrast with this, to keep the development performance constant by controlling the concentrations of compounds dissolving out of the light-sensitive material being processed. Accordingly, the concentrations of the former compounds are made higher than those in the color development tank solution, and the concentrations of the latter compounds are made lower than those in the color development tank solution.
- Examples of the former compounds include a color-developing agent and a preservative, and they are contained in the replenisher in amounts generally 1.1 to 2 times those in the tank solution.
- Examples of the latter compounds include a development inhibitor, represented by a halide (e.g. potassium bromide), and they are contained in the replenisher in amounts generally 0 to 0.6 times those of the tank solution.
- the concentration of the halide in the replenisher is generally 0.006 mol/liter or less, but it is required that the lower the replenishment rate is made, the more the concentration is decreased, and in some cases, the halide concentration is nil.
- compounds whose concentrations are hardly to change in the processing or with time are generally contained in the replenisher approximately in the same concentrations as those in the color-development tank solution.
- examples of such compounds are chelating agents and buffers.
- the pH of the color-development replenisher is generally made higher than that of the tank solution, by about 0.05 to 0.5, in order to prevent the pH of the tank solution from being lowered by the processing. It is required that the difference in this pH be made higher if the replenishment rate is to be lowered.
- the replenishment rate of the color developer is generally 3000 ml or less, preferably 100 ml to 1500 ml, and most preferably 100 to 600 ml, per square meter of the light-sensitive material.
- the processing temperature of the color developer is generally 20 to 55 °C, and preferably 30 to 50 °C.
- the processing time is suitably generally 20 sec to 5 min, preferably 30 sec to 3 min 30 sec, and more preferably 1 min to 3 min 20 sec.
- the color-developing bath is divided, if required, into two baths or more, and the replenishment with the color development replenisher may be made to the first bath or the last bath, to shorten the development time or to reduce further the replenishment rate.
- the color developer may be regenerated, to be used as a processing solution again, by processing the used color developer with an anion exchange resin, subjecting the used color developer to electrodialysis, or adding a processing chemical called a regenerating agent to the used color developer, to increase the activity of the color developer.
- the regeneration rate (the rate of the overflow in the replenisher) is preferably 50% or more, and particularly preferably 70% or more.
- the overflow of the color developer is regenerated, to be used as a color developer replenisher.
- an anion exchange resin is preferably used as a means for the regeneration.
- Particularly preferable compositions of anion exchange resins and methods for regenerating resins include those described in Diaion Manual (I), 14th edition (1986), published by Mitsubishi Chemical Industries Ltd.
- anionic exchange resins resins having compositions described in JP-A-2-952 and JP-A-1-281152 are preferable.
- the color-print-paper developer and the development replenisher contain a color-developing agent, and preferable examples are known aromatic primary amine color-developing agents, particularly p-phenylenediamine derivatives. Representative examples are shown below, but the present invention is not limited to them. Further, in recent years, among black-and-white light-sensitive materials, there are black-and-white light-sensitive materials wherein couplers are added to form black color, and a black and white image is formed by using a general-purpose usual color-developing solution. The color developing solution for use in the present invention can also be applied for the processing of this type of light-sensitive material.
- these p-phenylenediamine derivatives are particularly preferable, and among them Compounds 5) and 8) are preferable. Further, these p-phenylenediamine derivatives are generally in the form of sulfates, hydrochlorides, sulfites, and salts of naphthalenedisulfonic acid, p-toluenesulfonic acid, etc. when they are in the state of solid materials.
- the concentration of the aromatic primary amine developing agent in the developing solution or the replenisher is preferably 2 to 200 millimol, more preferably 12 to 200 millimol, and further more preferably 12 to 150 millimol, per liter of the developing solution, and the replenisher is designed to have a concentration higher than that of the developing solution due to the consumption in the development.
- a small amount of sulfite ions is contained in the developing solution, or the developing solution is substantially free from sulfite ions, in some cases.
- hydroxylamine is contained in the constitutional components of the composition, or it is not contained therein, in some cases. This is because hydroxylamine functions as a preservative of the developing solution, in addition to hydroxylamine itself having a silver development activity, and therefore this influences the photographic properties in some cases.
- the developer composition for use in the present invention preferably contain inorganic preservatives, such as a sulfite ion, and organic preservatives.
- inorganic preservatives refers generally to organic compounds that reduce the deterioration speed of the aromatic primary amine color-developing agent, when they are added to the processing solution of light-sensitive materials.
- organic preservatives are organic compounds that have a function of preventing color-developing agents from being oxidized with air or the like; and particularly effective organic preservatives are hydroxylamine derivatives, hydroxamic acids, hydrazides, phenols, ⁇ -hydroxyketones, ⁇ -aminoketones, saccharides, monoamines, diamines, polyamines, quaternary ammonium salts, nitroxy radicals, alcohols, oximes, diamide compounds, and fused-ring-type amines.
- JP-A-63-4235 JP-A-63-30845, JP-A-63-21647, JP-A-63-44655, JP-A-63-53551, JP-A-63-43140, JP-A-63-56654, JP-A-63-58346, JP-A-63-43138, JP-A-63-146041, JP-A-63-44657, and JP-A-63-44656, US-A-3,615,503 and US-A-2,494,903, JP-A-52-143020, and JP-B-48-30496.
- preservatives that may be contained, if required, include, for example, various metals described in JP-A-57-44148 and JP-A-57-53749, salicylic acids described in JP-A-59-180588, alkanolamines described in JP-A-54-3532, polyethyleneimines described in JP-A-56-94349, and aromatic polyhydroxy compounds described in US-A-3,746,544.
- alkanolamines are effective to upgrade long term stability of a developer, a replenisher itself, and a composition in a condensed state to which the developer or the replenisher are provided as a processing agent.
- Alkanolamines particularly effective in improving the long-term stability are, for example, triisopropanolamine, diisopropanolamine, monoisopropanolamine, and diethanolamine, and among them triisopropanolamine is preferable.
- triethanolamines can be preferably used.
- the amount of the above alkanolamines to be added is generally 0.01 to 1 mol and preferably 0.02 to 0.2 mol, per liter of the processing solution.
- hydroxylamine derivatives such as substituted or unsubstituted dialkylhydroxylamines, for example, disulfoethylhydroxylamine and diethylhydroxylamine, or aromatic polyhydroxy compounds can be preferably added.
- hydroxylamine derivatives are particularly preferable and their details are described, for example, in JP-A-1-97953, JP-A-1-186939, JP-A-1-186940, and JP-A-1-187557.
- chloride ions may be added, if necessary, and in many cases, generally chloride ions are contained in an amount of 3.5 x 10 -2 to 1.5 x 10 -1 mol/liter, but since chloride ions are released generally as a by-product of the development into the developing solution, they are not required to be added into the replenisher in many cases.
- bromide ions With respect to the inclusion of bromide ions, the same thing as that of chloride ions can be applied.
- concentration of bromide ions is 1.0 x 10 -3 mol/liter or less.
- bromide ions are added to the development replenisher so that the bromide ion concentration may fall in that range.
- sodium chloride, potassium chloride, ammonium chloride, lithium chloride, nickel chloride, magnesium chloride, manganese chloride, or calcium chloride can be mentioned, with preference given to sodium chloride and potassium chloride.
- bromide-ion-supply substance sodium bromide, potassium bromide, ammonium bromide, lithium bromide, calcium bromide, magnesium bromide, manganese bromide, nickel bromide, cerium bromide, or thallium bromide can be mentioned, with preference given to potassium bromide and sodium bromide.
- the developing solution may contain a fluorescent whitening agent.
- the fluorescent whitening agent triazinyl-4,4-diaminostilbene compounds are preferable.
- stilbene fluorescent whitening agents can be added to the color-developing solution as well as to any of the desilvering solution or the light-sensitive material.
- the developing solution or the replenisher used in color-print materials preferably has a pH of 9.5 to 13.0, and more preferably 9.8 to 12.5. To retain the above pH, it is preferable to use various buffers. As a buffer, potassium carbonate and sodium carbonate can be used.
- buffers examples include carbonates, phosphates, borates, tetraborates, hydroxybenzoates, glycil salts, N,N-dimethylglycine salts, leucine salts, norleucine salts, guanine salts, 3,4-dihydroxyphenylalanine salts, alanine salts, aminobutyrates, 2-amino-2-methyl-1,3-propandiol salts, valine salts, proline salts, trishydroxyaminomethane salts, and lysine salts.
- carbonates, phosphates, tetraborates, and hydroxybenzoates have such advantages that they are excellent in buffering function at a high pH region in pH of 9.0 or over, and that when they are added to the color-developing solution, the photographic performance is not adversely affected (e.g. fog), and that they are low in cost, so that these buffers are particularly preferably used.
- these buffers include, in addition to sodium carbonate and potassium carbonate, sodium bicarbonate, potassium bicarbonate, trisodium phosphate, tripotassium phosphate, disodium phosphate, dipotassium phosphate, sodium borate, potassium borate, sodium tetraborate (borax), potassium tetraborate, sodium o-hydroxybenzoate (sodium salicylate), potassium o-hydroxybenzoate, sodium 5-sulfo-2-hydroxybenzoate (sodium 5-suofosalicylate), and potassium 5-sulfo-2-hydroxybenzoate (potassium 5-sulfosalicylate).
- the present invention is not limited to these compounds.
- the amount of the buffers to be added is preferably 0.04 to 2.0 mol/liter, and particularly preferably 0.1 to 0.4 mol/liter, assuming the amount to be the total of the buffers.
- another color-developing-solution component that is, for example, a precipitation-preventing agent against calcium and magnesium, or is an agent for improving stability of the color-developing solution
- various chelating agents can be used. Examples include nitrilotriacetic acid, diethylenetriaminepentaacetic acid, ethylenediaminetetraacetic acid, N,N,N-trimethylenephosphonic acid, ethylenediamine-N,N,N',N'-tetramethylenesulfonic acid, ethylenediaminN,N-disuccinic acid, N,N-di(carboxylate)-L-aspartic acid, ⁇ -alaninedisussinic acid, ehylenediamine-N,N,N',N'-tetramethylenesulfonic acid, transcyclohexane-diaminetetraacetic acid, 1,2-diaminopropanetetraacetic acid, glycol ether diamine
- Two or more of these chelating agents may be used in combination, if necessary.
- these chelating agents preferably the amount is enough to sequester the metal ions in the color-developing solution, and, generally, these chelating agents are used in a concentration in the developing solution or in the replenisher of 0.1 to 10 g per liter.
- any of development accelerators can be added, if necessary.
- thioether compounds disclosed, for example, in JP-B-37-16088, JP-B-37-5987, JP-B-38-7826, JP-B-44-12380, JP-B-45-9019, and US-A-3 813 247; p-phenylenediamine compounds disclosed in JP-A-52-49829 and JP-A-50-15554, quaternary ammonium salts disclosed, for example, in JP-A-50-137726, JP-B-44-30074, JP-A-56-156826, and JP-A-52-43429; amine compounds described, for example, in US-A-2 494 903, US-A-3 128 182, US-A-4 230 796, US-A-3 253 919, JP-B-41-11431, US-A-2 482 546, US-A-2 596 926, and US-A-3 582 346; polyalkylene oxides disclosed, for example, in JP-B-37-
- an arbitrary antifoggant can be added.
- the said alkali metal halide such as sodium chloride, potassium bromide, and potassium iodide
- an organic antifoggant can be used.
- the organic antifoggant include nitrogen-containing heterocyclic compounds, such as benzotriazole, 6-nitrobenzimidazole, 5-nitroisoindazole, 5-methylbenzotriazole, 5-nitrobenzotriazole, 5-chlorobenzotriazole, 2-thiazolyl-benzimidazole, 2-thiazolylmethyl-benzimidazole, indazole, hydroxyazaindolidine, and adenine.
- surfactants include, for example, compounds of formula (I) or (II) described in JP-A-4-195037, and compounds of any of formulas (I) to (X) described in JP-A-4-81750.
- the surface tension of the color-developing solution and the color development replenisher is brought to 20 to 60 dyn/cm.
- the processing temperature at the color-development in the present invention is generally 30 to 55 °C, preferably 35 to 55 °C, and more preferably 38 to 45 °C.
- the development processing time is generally 5 to 90 sec, and preferably 15 to 60 sec, and the method of the present invention is suit to the extremely rapid processing of 10 to 30 sec.
- the replenishing rate is generally 20 to 600 ml, preferably 30 to 120 ml, and particularly preferably 15 to 60 ml, per m 2 of the photographic material.
- the light-sensitive material that has been processed with the bleaching solution is processed with a processing solution having a fixing capacity.
- the processing solution having a fixing capacity means specifically a fixing solution and a bleach-fix solution.
- the bleaching agent of the bleaching solution and the bleaching agent of the bleach-fix solution are the same or different.
- a washing step may be provided prior to the processing with the bleach-fix solution.
- the processing solution having a fixing capacity contains a fixing agent.
- a fixing agent can be mentioned thiosulfates, such as sodium thiosulfate, ammonium thiosulfate, sodium ammonium thiosulfate, and potassium thiosulfate, thiocyanates (rhodanates), such as sodium thiocyanate, ammonium thiocyanate, and potassium thiocyanate, thiourea, and thioethers.
- Ammonium thiosulfate is particularly preferably used inter alia.
- the amount of the fixing agent is generally 0.3 to 3 mol and preferably 0.5 to 2 mol, per liter of the processing solution having a fixing capacity.
- a thiosulfate in combination with ammonium thiocyanate (ammonium rhodanate), thiourea, a thioether (e.g. 3,6-dithia-1,8-octanediol), or a thiosulfonic acid (e.g. ammonium methanethiosulfonate).
- ammonium thiocyanate ammonium rhodanate
- thiourea e.g. 3,6-dithia-1,8-octanediol
- a thiosulfonic acid e.g. ammonium methanethiosulfonate
- a combination of ammonium thiosulfate with ammonium methanethiosulfonate is preferable.
- the amount of these compounds used in combination is generally 0.01 to 1 mol and preferably 0.1 to 0.5 mol, per liter of the processing solution having a fixing capacity, but in the case of a thiocyanate, the use of 1 to 3 mol can increase the fixing acceleration effect considerably.
- a thiosulfonic acid preferably the below-described sulfinic acid is used additionally.
- the processing solution having a fixing capacity can contain, as preservatives, sulfites (e.g. sodium sulfite, potassium sulfite, and ammonium sulfite), hydroxylamines, hydrazines, bisulfite-addition compounds of aldehyde compounds (e.g. acetaldehyde sodium bisulfite and particularly preferably compounds described in Japanese patent application No. 1-298935), or sulfinic acid compounds described in JP-A-1-231051. Further, various fluorescent whitening agents, anti-foaming agents, surfactants, polyvinyl pyrrolidones, and organic solvents, such as methanol, can be contained.
- sulfites e.g. sodium sulfite, potassium sulfite, and ammonium sulfite
- hydroxylamines e.g. sodium sulfite, potassium sulfite, and ammonium sulfite
- chelating agents such as various aminopolycarboxylic acids and organic phosphonic acids, are preferably added in order to stabilize the processing solution.
- chelating agents can be mentioned, for example, 1-hydroxyethylidene-1,1-diphosphonic acid, ethylenediamine-N,N,N',N'-tetramethylenephosphonic acid, nitrilotrimethylenephosphonic acid, ethylenediaminetetraacetic acid, diethylenetriaminepentaacetic acid, cyclohexanediaminetetraacetic acid, 1,2-propylenediaminetetraacetic acid, and 1,3-diaminopropanetetraaectic acid.
- 1-hydroxyethylidene-1,1-diphosphonic acid, 1,3-diaminopropanetetraacetic acid, and ethylenediaminetetraacetic acid are particularly preferable.
- the amount of the chelating agent to be added is generally 0.01 to 0.3 mol and preferably 0.03 to 0.2 mol, per liter of the processing solution.
- the pH of the fixing solution is preferably 5 to 9 and more preferably 6 to 8. Further, the pH of the bleach-fix solution is preferably 4.0 to 7.0 and more preferably 5.0 to 6.5.
- a compound having a pKa in the range of 6.0 to 9.0 is preferably contained as a buffer.
- imidazoles such as imidazole and 2-methyl-imidazole, are preferable.
- the amount of the compound to be added is preferably 0.1 to 10 mol and more preferably 0.2 to 3 mol, per liter of the processing solution.
- the bleach-fix solution can contain the above-described compounds that can be contained in the bleaching solution.
- the bleach-fix solution (start solution) at the start of the processing is prepared by dissolving in water the above-described compounds that are to be used in the bleach-fix solution, or it may be prepared by mixing suitable amounts of a bleaching solution and a fixing solution that are prepared separately.
- the replenishment rate of the fixing solution or the bleach-fix solution in the case of the use of a replenishing system is preferably 100 to 3,000 ml and more preferably 300 to 1,800 ml, per square meter of the light-sensitive material, in the case of color photographing materials.
- the above replenishment rate is generally 20 to 1,500 ml, preferably 30 to 600 ml, and more preferably 30 to 200 ml, per square meter of the light-sensitive material, in the case of color print materials.
- the replenishment with the bleach-fix solution may be carried out by the replenishment with a bleach-fix replenisher, or by using the overflow of the fixing solution and the bleaching solution, as described in JP-A-61-143755 or Japanese patent application No. 2-216389.
- the total processing time of the processing having a fixing capacity is generally 0.5 to 5 min, preferably 1.5 to 4 min, and particularly preferably 2 to 3.5 min, in the case of color photographing materials.
- the above total processing time is generally 5 sec to 2 min, preferably 10 sec to 1 min 40 sec, and more preferably 10 sec to 45 sec, in the case of color print materials.
- the processing temperature of the processing solution having a fixing capacity for use in the present invention is generally 25 to 50 °C and preferably 35 to 45 °C.
- silver can be recovered in the known manner, and the solution obtained by recovering the silver can be used for a regenerated solution.
- the solution having a fixing capacity in the case wherein silver is recovered is preferably the fixing solution.
- an electrolysis method described in FR-A-2 299 667
- a precipitation method described in JP-A-52-73037 or German patent No. 2,331,220
- an ion exchange method JP-A-51-17114 and German patent No. 2,548,237)
- a metal replacement method GB-A-1 353 805
- these silver recovering methods are carried out in an inline manner from the tank solution, because in that case the rapid processibility becomes more favorable.
- the concentration of silver in the solution having a fixing capacity is kept at generally 3 g/liter or less, and preferably 1 g/liter or less.
- the replenishment rate of the solution having a fixing capacity can be further reduced, and it is preferably 100 to 300 ml per square meter of the light-sensitive material in the case of color photographing materials.
- a processing step of washing, stabilizing, or the like that is generally carried out may be performed.
- a simple processing method wherein stabilizing is carried out without carrying out substantial washing can be used.
- the washing water used in the washing step may contain various surface-active agents, to prevent the processed light-sensitive material from being dried unevenly due to water droplets.
- the surface-active agents include polyethylene glycol-type nonionic surface-active agents, polyhydric alcohol-type nonionic surface-active agents, alkylbenzenesulfonate-type anionic surface-active agents, higher alcohol sulfate-type anionic surface-active agents, alkylnaphthalenesulfonate-type anionic surface-active agents, quaternary ammonium salt-type cationic surface-active agents, amine salt-type cationic surface-active agents, amino salt-type amphoteric surface-active agents, and betaine-type amphoteric surface-active agents.
- nonionic surface-active agents are preferably used, with particular preference given to alkylphenol ethylene oxide adducts.
- the alkylphenol is particularly preferably octylphenol, nonylphenol, dodecylphenol, or dinonylphenol, and the addition molar number of ethylene oxide is particularly preferably 8 to 14 (mol).
- a silicon-series surface-active agent high in antifoaming effect is also preferably used.
- the washing water can contain a variety of bacteria-proofing agents and mildew-proofing agents, to prevent the formation of scale or the existence of mildew occurring on processed light-sensitive materials.
- bacteria-proofing agents and mildew-proofing agents can be used, for example, one or more of thiazorilbenzoimidazole compounds, as described in JP-A-57-157244 and JP-A-58-105145, isothiazolone compounds, as described in JP-A-57-8542, and general-purpose mildew-proofing agents described in " Journal Antibacteria and Antifungus Agents ,” Vol. 1, No.
- pp 207 to 223 (1983) such as chlorophenol compounds, represented by trichlorophenol; bromophenol compounds, organotin compounds, organozinc compounds, thiocyanic acid compounds, isothiocyanic acid compounds, acid amide compounds, diazine compounds, triazine compounds, thiourea compounds, benzotriazolealkylguanidine compounds, quaternary ammonium salts, represented by benzalkonium chloride; or antibiotics, such as penicillins.
- various fungicides described in JP-A-48-83820 can be used.
- chelating agents are additionally used.
- chelating agents include, for example, aminopolycarboxylic acids, such as ethylenediaminetetraacetic acid and diethylenetriaminepentaacetic acid, organic phosphonic acids, such as 1-hydroxyethylidene-1,1-diphosphonic acid and ethylenediamine-N,N,N',N'-tetramethylenephosphonic acid, and hydrolyzates of maleic anhydride polymers, as described in EP-A-345 172 (A1).
- aminopolycarboxylic acids such as ethylenediaminetetraacetic acid and diethylenetriaminepentaacetic acid
- organic phosphonic acids such as 1-hydroxyethylidene-1,1-diphosphonic acid and ethylenediamine-N,N,N',N'-tetramethylenephosphonic acid
- hydrolyzates of maleic anhydride polymers as described in EP-A-345 172 (A1).
- the above preservatives that can be contained in the fixing solution or the bleach-fix solution are preferably contained in the washing water.
- the stabilizing solution used in the stabilizing step is a processing solution for stabilizing dye images.
- a solution having a buffering function in the pH range of 3 to 6 such as a solution containing an aldehyde (e.g. formalin) can be used.
- an aldehyde e.g. formalin
- stabilizing solutions preferably used in the present invention are described.
- the stabilizing solution is substantially free from formaldehyde.
- substantially free from formaldehyde means that the total amount of free formaldehyde and its hydrate is 0.003 mol or less, per liter of the stabilizing solution.
- a formaldehyde vapor can be restrained from being scattered at the time of the processing.
- a formaldehyde-releasing compound is allowed to exist in the stabilizing solution, the bleaching solution, or a bath preceding it (e.g. an adjusting bath).
- formaldehyde-releasing compound hexamethylenetetramine and its derivatives, formaldehyde-bisulfite adducts, azolylmethylamines, and N-methylol compounds.
- hexamethylenetetramine and its derivatives those compounds described in "Beilsteins Handbuch der Organishen Chemie," No. II enlarged edition, Vol. 26, pages 200 to 212 can be used, with particular preference given to hexamethylenetetramine.
- formaldehyde-bisulfite adducts formaldehyde-sodium bisulfite is preferable.
- azolylmethylamines those obtained by reacting three compounds, i.e., an azole selected from among triazole, pyrazole, and imidazole, an amine selected from piperazine, morpholine, 4-hydroxyethylpiperidine, and 4-hydroxypiperidine, and formaldehyde are preferable.
- an azole selected from among triazole, pyrazole, and imidazole an amine selected from piperazine, morpholine, 4-hydroxyethylpiperidine, and 4-hydroxypiperidine, and formaldehyde
- N,N'-bis(1,2,4-triazol-1-ylmethyl)piperazine and N,N'-bis(pyrazol-1-ylmethyl)piperazine are preferable.
- N-methylol compounds particularly pyrazole and N-methylol compounds that are derivatives thereof, triazole and N-methylol compounds that are derivatives thereof, and urazol and N-methylol compounds that are derivatives thereof are preferable.
- N-methylol compounds include 1-hydroxymethylpyrazole, 1-hydroxymethyltriazole, and 1-hydroxymethylurazol.
- the most preferable one is 1-hydroxymethylpyrazole.
- N-methylol compounds can be synthesized easily by reacting an amine compound having no methylol group with formaldehyde or paraformaldehyde.
- formaldehyde-releasing compounds particularly preferable ones are hexamethylenetetramine, formaldehyde-sodium bisulfite, and the above preferable azolylmethylamines and N-methylol compounds.
- N,N'-bis(1,2,4-triazol-1-ylmethyl)piperazine and N,N'-bis(pyrazol-1-ylmethyl)piperazine are most preferable.
- an amine compound such as triazole or pyrazole
- an amine compound such as triazole or pyrazole
- a preferable amount of the above formaldehyde-releasing compound to be added is 0.003 to 0.2 mol and preferably 0.005 to 0.05 mol, per liter of the processing solution.
- These formaldehyde-releasing compounds may be used in combination of two or more in the bath.
- the stabilizing solution can contain all compounds that can be added to the washing water, as well as ammonium compounds (e.g. ammonium chloride, ammonium sulfite), metal compounds (e.g. a bismuth compound, an aluminum compound), a fluorescent-whitening agent, a hardener; alkanolamines, as described in US-A-4,786,583, according to the occasion.
- ammonium compounds e.g. ammonium chloride, ammonium sulfite
- metal compounds e.g. a bismuth compound, an aluminum compound
- a fluorescent-whitening agent e.g. a bismuth compound, an aluminum compound
- a hardener e.g. a bismuth compound, an aluminum compound
- alkanolamines as described in US-A-4,786,583, according to the occasion.
- the washing step and the stabilizing step are preferably of a multi-stage counter current system, and the number of stages is preferably 2 to 4.
- the replenishment rate is generally 1 to 50 times, preferably 2 to 30 times, and more preferably 2 to 15 times, the amount carried in from the preceding bath per unit area.
- water used in the washing step or the stabilizing step besides tap water, water deionized with ion exchange resins to bring the concentrations of Ca and Mg to 5 mg/liter or below, or water sterilized with a halogen lamp, an ultraviolet germicidal lamp, or the like, is preferably used.
- water to supplement the evaporation in the processing solutions tap water can be used, but deionized water or sterilized water preferably used in the washing step or the stabilizing step, is preferably used.
- the overflow of the washing step or the stabilizing step may be flowed into the preceding bath, that is, the bath having a fixing capacity, to reduce the amount of waste liquor.
- the developing apparatus for carrying out the present invention
- the stirring method, the materials, etc. of the developing apparatus are preferably those described in JP-A-4-130432.
- Examples of the silver halide color photographic light-sensitive material to which the present invention is preferably applied includes photographing-light-sensitive materials, such as color reversal films and color negative films having a silver bromoiodide emulsion applied, and print light-sensitive materials, such as color print papers, with particular preference given to color negative films and, inter alia, those having a magnetic recording layer on a base.
- photographing-light-sensitive materials such as color reversal films and color negative films having a silver bromoiodide emulsion applied
- print light-sensitive materials such as color print papers, with particular preference given to color negative films and, inter alia, those having a magnetic recording layer on a base.
- the photographing light-sensitive materials those having a coating amount of silver of about 3 to 8 g/m 2 are preferably used, and for the halogen composition of the silver halide emulsion, silver bromoiodide (whose silver iodide content is 3 to 10 mol%) is preferable.
- the print light-sensitive material those having a coating amount of silver of 1 g/m 2 or less, and particularly preferably 0.3 to 0.8 g/m 2 , are preferably used, and for the silver halide composition of the silver halide emulsion, high-silver chloride is preferable.
- the magnetic recording layer is a layer formed by coating on a base with an aqueous or organic solvent coating solution containing magnetic particles dispersed in a binder.
- a ferromagnetic iron oxide such as ⁇ Fe 2 O 3 , Co-coated ⁇ Fe 2 O 3 , Co-coated magnetite, Co-containing magnetite, ferromagnetic chromium dioxide, a ferromagnetic metal, a ferromagnetic alloy, hexagonal Ba ferrite, Sr ferrite, Pb ferrite, and Ca ferrite.
- a Co-coated ferromagnetic iron oxide, such as Co-coated ⁇ Fe 2 O 3 is preferable.
- the shape may be any of a needle shape, a rice grain shape, a spherical shape, a cubic shape, a plate-like shape, and the like.
- the specific surface area is preferably 20 m 2 /g or more, and particularly preferably 30 m 2 /g or more, in terms of S BET .
- the saturation magnetization ( ⁇ s) of the ferromagnetic material is preferably 3.0 x 10 4 to 3.0 x 10 5 A/m, and particularly preferably 4.0 x 10 4 to 2.5 x 10 5 A/m.
- the ferromagnetic particles may be surface-treated with silica and/or alumina or an organic material.
- the surface of the magnetic particles may be treated with a silane coupling agent or a titanium coupling agent, as described in JP-A-6-161032. Further, magnetic particles whose surface is coated with an inorganic or an organic material, as described in JP-A-4-259911 and 5-81652, can be used.
- thermoplastic resin As the binder used for the magnetic particles, as described in JP-A-4-219569, a thermoplastic resin, a thermal-setting resin, a radiation-setting resin, a reactive resin, an acid-degradable polymer, an alkali-degradable polymer, a biodegradable polymer, a natural polymer (e.g. a cellulose derivative and a saccharide derivative), and a mixture of these can be used.
- the above resins generally have a glass transition temperature Tg of -40 to 300 °C and a weight-average molecular weight of 2,000 to 1,000,000.
- Examples include vinyl copolymers, cellulose derivatives, such as cellulose diacetates, cellulose triacetates, cellulose acetate propionates, cellulose acetate butylates, and cellulose tripropionates; acrylic resins, and polyvinyl acetal resins; and gelatin is also preferable. Cellulose di(tri)acetates are particularly preferable.
- To the binder may be added an epoxy, aziridine, or isocyanate crosslinking agent, to harden the binder.
- isocyanate crosslinking agent examples include isocyanates, such as tolylene diisocyanate, 4,4'-diphenylmethane diisocyanate, hexamethylene diisocyanate, and xylylene diisocyanate; reaction products of these isocyanates with polyalcohols (e.g. a reaction product of 3 mol of tolylene diisocyanate with 1 mol of trimethylolpropane), and polyisocyanates produced by condensation of these isocyanates, which are described, for example, in JP-A-6-59357.
- isocyanates such as tolylene diisocyanate, 4,4'-diphenylmethane diisocyanate, hexamethylene diisocyanate, and xylylene diisocyanate
- reaction products of these isocyanates with polyalcohols e.g. a reaction product of 3 mol of tolylene diisocyanate with 1 mol of trimethylolpropane
- the method of dispersing the foregoing magnetic material in the foregoing binder is preferably one described in JP-A-6-35092, in which method use is made of a kneader, a pin-type mill, an annular-type mill, and the like, which may be used alone or in combination.
- a dispersant described in JP-A-5-088283 and other known dispersants can be used.
- the thickness of the magnetic recording layer is generally 0.1 to 10 ⁇ m, preferably 0.2 to 5 ⁇ m, and more preferably 0.3 to 3 ⁇ m.
- the weight ratio of the magnetic particles to the binder is preferably from (0.5:100) to (60:100), and more preferably from (1:100) to (30:100).
- the coating amount of the magnetic particles is generally 0.005 to 3 g/m 2 , preferably 0.01 to 2 g/m 2 , and more preferably 0.02 to 0.5 g/m 2 .
- the magnetic recording layer used in the present invention can be provided to the undersurface of the photographic base by coating or printing through all parts or in a striped fashion.
- To apply the magnetic recording layer use can be made of an air doctor, a blade, an air knife, squeezing, impregnation, a reverse roll, a transfer roll, gravure, kiss, cast, spraying, dipping, a bar, extrusion, or the like.
- a coating solution described, for example, in JP-A-5-341436 is preferable.
- the magnetic recording layer may be provided with functions, for example, of improving lubricity, of regulating curling, of preventing electrification and adhesion, and of abrading a head, or it may be provided with another functional layer that is provided with these functions.
- the aspherical inorganic particles preferably comprise a fine powder of an oxide, such as aluminum oxide, chromium oxide, silicon dioxide, and titanium dioxide; a carbide, such as silicon carbide and titanium carbide; diamond, or the like.
- the surface of these abrasives may be treated with a silane coupling agent or a titanium coupling agent.
- These particles may be added to the magnetic recording layer, or they may form an overcoat (e.g. a protective layer and a lubricant layer) on the magnetic recording layer.
- an overcoat e.g. a protective layer and a lubricant layer
- the above-mentioned binders can be used, and preferably the same binder as used in the magnetic recording layer is used.
- Light-sensitive materials having a magnetic recording layer are described in US-A-5 336 589, 5 250 404, 5 229 259, and 5 215 874, and EP-466 130.
- the light-sensitive material that is processed by the present invention is preferably a light-sensitive material for photographing (shooting), and its base is preferably a polyester base.
- Polyester bases for use in the present invention are described in detail in Kokaigiho, Kogi No. 94-6023 (Hatsumei-kyokai; 15, 3, 1994) in detail.
- Polyesters for use in the present invention are produced by using, as essential components, diols and aromatic dicarboxylic acids.
- aromatic dicarboxylic acids include 2,6-, 1,5-, 1,4- and 2,7-naphthalene dicarboxylic acids; terephthalic acid, isophthalic acid, and phthalic acid; and examples of the diols include diethylene glycol, triethylene glycol, cyclohexanedimethanol, bisphenol A, and bisphenols.
- Examples of their polymers include homopolymers, such as polyethylene terephthlates, polyethylene naphthalates, and polycyclohexanedimethanol terephthalates.
- Polyesters comprising 2,6-naphthalenedicarboxylic acid as an acidic reaction component, at a content of 50 to 100 mol% of the total dicarboxylic acid component, are particularly preferable. Among them, polyethylene 2,6-naphthalates are particularly preferable. The average molecular weight is in the range of generally about 5,000 to 200,000.
- the Tg of the polyesters for use in the present invention is generally 50 °C or over, and preferably 90 °C or over.
- the polyester base is heat-treated at a heat treatment temperature of generally 40 °C or over, but less than the Tg, and preferably at a heat treatment temperature of the Tg - 20 °C or more, but less than the Tg, so that it will hardly have core set curl.
- the heat treatment may be carried out at a constant temperature in the above temperature range, or it may be carried out with cooling.
- the heat treatment time is generally 0.1 hours or more, but 1,500 hours or less, and preferably 0.5 hours or more, but 200 hours or less.
- the heat treatment of the base may be carried out with the base rolled, or it may be carried out with it being conveyed in the form of web.
- the surface of the base may be made rough (unevenness, for example, by applying electroconductive inorganic fine particles, such as SnO 2 and Sb 2 O 5 ), so that the surface state may be improved. Further, it is desirable to provide, for example, a rollette (knurling) at the both ends for the width of the base (both right and left ends towards the direction of rolling) to increase the thickness only at the ends, so that a trouble of deformation of the base will be prevented.
- the trouble of deformation of the base means that, when a base is wound on a core, on its second and further winding, the base follows unevenness of its cut edge of the first winding, deforming its flat film-shape.
- heat treatments may be carried out at any stage after the production of the base film, after the surface treatment, after the coating of a backing layer (e.g. with an antistatic agent and a slipping agent), and after coating of an undercoat, with preference given to after coating of an antistatic agent.
- a backing layer e.g. with an antistatic agent and a slipping agent
- an undercoat e.g. with an antistatic agent and a slipping agent
- polyester may be blended (kneaded) an ultraviolet absorber. Further, prevention of light piping can be attained by blending dyes or pigments commercially available for polyesters, such as Diaresin (trade name, manufactured by Mitsubisi Chemical Industries Ltd.), and Kayaset (trade name, manufactured by Nippon Kayaku Co., Ltd.).
- Diaresin trade name, manufactured by Mitsubisi Chemical Industries Ltd.
- Kayaset trade name, manufactured by Nippon Kayaku Co., Ltd.
- a surface treatment is preferably carried out.
- a surface activation treatment can be mentioned, which includes a chemical treatment, a mechanical treatment, a corona discharge treatment, a flame treatment, an ultraviolet treatment, a high-frequency treatment, a glow discharge treatment, an active-plasma treatment, a laser treatment, a mixed-acid treatment, and an ozone oxidation treatment.
- an ultraviolet irradiation treatment, a flame treatment, a corona treatment, and a grow treatment are preferable.
- a single layer or two or more layers may be used.
- the binder for the undercoat layer for example, copolymers produced by using, as a starting material, a monomer selected from among vinyl chloride, vinylidene chloride, butadiene, methacrylic acid, acrylic acid, itaconic acid, maleic anhydride, and the like, as well as polyethylene imines, epoxy resins, grafted gelatins, nitrocelluloses, and gelatin, can be mentioned.
- compounds that can swell the base resorcin and p-chlorophenol can be mentioned.
- gelatin hardening agents in the undercoat layer chrome salts (e.g.
- chrome alum chrome alum
- aldehydes e.g. formaldehyde and glutaraldehyde
- isocyanates active halogen compounds (e.g. 2,4-dichloro-6-hydroxy-s-triazine), epichlorohydrin resins, active vinyl sulfone compounds, and the like
- active halogen compounds e.g. 2,4-dichloro-6-hydroxy-s-triazine
- epichlorohydrin resins active vinyl sulfone compounds, and the like
- SiO 2 TiO 2
- inorganic fine particles e.g. 2,4-dichloro-6-hydroxy-s-triazine
- epichlorohydrin resins e.g. 2,4-dichloro-6-hydroxy-s-triazine
- epichlorohydrin resins e.g. 2,4-dichloro-6-hydroxy-s-triazine
- epichlorohydrin resins e.g
- an antistatic agent is preferably used.
- the antistatic agent polymers, including carboxylic acids, carboxylates, and sulfonates; cationic polymers, and ionic surface-active compounds can be mentioned.
- Most preferable antistatic agents are fine particles of at least one crystalline metal oxide selected from the group consisting of ZnO, TiO 2 , SnO 2 , Al 2 O 3 , In 2 O 3 , SiO 2 , MgO, BaO, MoO 3 , and V 2 O 5 , and having a specific volume resistance of 10 7 ⁇ cm or less, and more preferably 10 5 ⁇ cm or less and a particle size of 0.001 to 1.0 ⁇ m, or fine particles of their composite oxides (Sb, P, B, In, S, Si, C, etc.); as well as fine particles of the above metal oxides in the form of a sol, or fine particles of composite oxides of these.
- crystalline metal oxide selected from the group consisting of ZnO, TiO 2 , SnO 2 , Al 2 O 3 , In 2 O 3 , SiO 2 , MgO, BaO, MoO 3 , and V 2 O 5 , and having a specific volume resistance of 10 7 ⁇ cm
- the content thereof in the light-sensitive material is preferably 5 to 500 mg/m 2 , and particularly preferably 10 to 350 mg/m 2 .
- the ratio of the amount of the electroconductive crystalline oxide or its composite oxide to the amount of the binder is preferably from 1/300 to 100/1, and more preferably from 1/100 to 100/5.
- the light-sensitive material for use in the present invention preferably has slipperiness.
- the slipping-agent-containing layer is provided on both the side of the light-sensitive layer, and the side of the backing layer.
- Preferable slipperiness is 0.25 or less, but 0.01 or more, in terms of coefficient of dynamic friction. In this case, the value is obtained in the measurement wherein a sample is transferred at 60 cm/min against a stainless steel ball of a diameter 5 mm, at 25 °C and 60% RH. In this evaluation, if it is replaced with the light-sensitive layer surface as the partner material, the value will be almost on the same level.
- Examples of the slipping agent that can be used in the present invention include, for example, polyorganosiloxanes, higher fatty acid amides, higher fatty acid metal salts, and esters of higher fatty acids with higher alcohols; and polyorganosiloxanes that can be used include polydimethylsiloxane, polydiethylsiloxane, polystyrylmethylsiloxane, and polymethylphenylsiloxane.
- the layer to which the slipping agent is added is preferably the outermost layer of the light-sensitive emulsion layers, or the backing layer.
- polydimethylsiloxanes, and esters having a long-chain alkyl group are preferable.
- the light-sensitive material for use in the present invention preferably have a matting agent.
- the matting agent may be added to either the side of the light-sensitive emulsions or the side of the backing layer, and particularly preferably it is added to the outermost layer on the side of the light-sensitive emulsions.
- the matting agent may or may not be soluble in the processing solution, and preferably a matting agent soluble in the processing solution and a matting agent insoluble in the processing solution are used together.
- the particle diameter is 0.8 to 10 ⁇ m. The narrower the particle diameter distribution is, the more preferable it is.
- Preferably 90% or more of all the particles is within 0.9 to 1.1 times the average particle diameter.
- the light-sensitive materials used in the present invention are preferably those described in JP-A-4-125558, from page 14, upper left column, line 1, to page 18, lower left column, line 11.
- a silver bromoiodide emulsion having an average silver iodide content of 3 to 20 mol% is preferable, whose silver halide grains are preferably tabular grains having an aspect ratio of 5 or more, or double-structure grains wherein the inside and the outside are different in halogen composition.
- the grains may be ones wherein the inside and the outside constitute clear layer structures.
- the aspect ratio is preferably from 5 to 20, and more preferably from 6 to 12.
- the light-sensitive material used in the present invention has preferably a layer containing a non-light-sensitive fine grain silver halide having an average grain diameter of 0.02 to 0.2 ⁇ m.
- the fine grain silver halide is made preferably of silver bromide having a silver iodide content of 0.5 to 10 mol%.
- Additives used in the light-sensitive material for use in the present invention are described below.
- Additive RD 17643 RD 18716 RD 307105 1 Chemical sensitizers p.23 p.648 (right column) p.866 2 Sensitivity-enhancing agents _ p.648 (right column) - 3 Spectral sensitizers and Supersensitizers pp.23-24 pp.648 (right column) -649 (right column) pp.866-868 4 Brightening agents p.24 p.648 (right column) p.868 5 Light absorbers, Filter dyes, and UV Absorbers pp.25-26 pp.649 (right column) -650 (left column) P.873 6 Binders p.26 p.651 (left column) pp.873-874 7 Plasticizers and Lubricants p.27 p.650 (right column) p.876 8 Coating aids and Surface-active agents pp.26
- various dye-forming couplers can be used, and particularly preferable couplers are the following:
- couplers whose color-formed dyes have suitable diffusibility those described in US-A-4 366 237, GB 2 125 570, EP-B-96,873, and DE 3,234,533 are preferable.
- Couplers for correcting undesired absorption of color-formed dyes are preferably yellow-colored cyan couplers represented by formula (CI), (CII), (CIII), or (CIV) (particularly YC-86 on page 84) described in EP-A-456,257(A1), page 5; yellow-colored magenta couplers ExM-7 (page 202), EX-1 (page 249), and EX-7 (page 251) described in EP-A-456,257(A1); magenta-colored cyan couplers CC-9 (column 8) and CC-13 (column 10) described in US-A-4 833 069; (2) (column 8) of US-A-4 837 136; and colorless masking couplers (particularly, exemplified compounds on pages 36 to 45) represented by formula (A) in claim 1 of WO 92/11575.
- containers e.g. film patrones (magazines)
- the major material of the patrone to be used may be metal or synthetic plastic, with preference given to plastic materials, such as polystyrenes, polyethylenes, polypropylenes, polyphenyl ethers, and the like.
- the patrone for use in the present invention may contain various antistatic agents, and preferably, for example, carbon black, metal oxide particles; nonionic, anionic, cationic, and betaine surface-active agents, or polymers can be used.
- antistatic patrones are described in JP-A-1-312537 and JP-A-1-312538.
- the resistance of the patrone at 25 °C and 25% RH is preferably 10 12 ⁇ or less.
- plastic patrones are made of plastics with which carbon black or a pigment has been kneaded, to make the patrones screen light.
- the size of the patrone may be size 135, that is currently used, and, to make cameras small, it is effective to change the diameter of the 25-mm cartridge of the current size 135, to 22 mm or less.
- the volume of the case of the patrone is 30 cm 3 or less, and more preferably 25 cm 3 or less.
- the weight of the plastic to be used for the patrone or the patrone case is preferably 5 to 15 g.
- the patrone may be one in which a spool is rotated to deliver a film.
- the structure may be such that the forward end of film is housed in the patrone body, and by rotating a spool shaft in the delivering direction, the forward end of the film is delivered out from a port of the patrone.
- film formats are preferably those as described in "FUJIFILM ADVANCED PHOTO SYSTEM LAB SYSTEM GUIDE,” pages 3 to 5, published by Fuji Photo Film Co., Ltd., wherein a light-sensitive material having a film width of 24 mm and provided with a magnetic recording function is housed in a plastic small-sized cartridge.
- the light-sensitive material for use in the present invention can contain compounds described in JP-A-60-107029, JP-A-60-252340, JP-A-1-44940, and JP-A-1-45687 that can undergo the oxidation-reduction reaction with the oxidized product of a developing agent to release a fogging agent, a development accelerator, a silver halide solvent, etc.
- the light-sensitive material for use in the present invention contains mercapto compounds described, for example, in US-A-4 740 454, JP-A-62-018539, US-A-4 788 132, and JP-A-1-283551.
- the light-sensitive material for use in the present invention can contain compounds described, for example, in JP-A-1-106052 that release a fogging agent, a development accelerator, a silver halide solvent, or their precursor independently of the amount of developed silver resulting from development processing.
- the light-sensitive material for use in the present invention can be preferably contained dyes that are dispersed by methods described in International Publication No. WO 88/04794 and JP-T-1-502912 ("JP-T” means a published searched patent publication), and dyes described, for example, in European Patent EP-0,317,308 (A2), US-A-4 420 555, and JP-A-1-259358.
- various antiseptics and mildewproofing agents such as n-butyl, p-hydroxybenzoate, phenol, 4-chloro-3,5-dimethylphenol, 2-phenoxyethanol, 2-(4-thiazolyl)benzimidazole, and 1,2-benzisothiazolin-3-on, as described in JP-A-63-257747, JP-A-62-272248, and JP-A-1-80941, and phenetyl alcohol.
- light-sensitive materials that can be subjected to C-41 processing of Eastman Kodak Co. or CN-16 processing of Fuji Photo Film Co., Ltd. are preferably used, such as
- Light-sensitive materials for color photographic prints to which the present invention is applied are described.
- the method of the present invention can be applied to light-sensitive materials for both amateurs and professionals.
- the method of the present invention can also effectively be applied to silver halide color photographic light-sensitive materials containing a pyrrolotriazole derivative as a cyan coupler.
- a pyrrolotriazole derivative as cyan couplers.
- the use of pyrrolotriazole derivatives as cyan couplers is disclosed, for example, in JP-A-5-150423, JP-A-5-255333, JP-A-202004, JP-A-7-48376, and JP-A-9-189988.
- the light-sensitive silver halide emulsion in the light-sensitive material as a positive material, such as a color paper is preferably made up of silver halide grains that have a silver chloride content of at least 95 mol% with the rest being silver bromide and are substantially free from silver iodide.
- the term "substantially free from silver iodide” means that the silver iodide content is generally 1 mol% or less, preferably 0.2 mol% or less, and more preferably 0 mol%.
- the above silver halide emulsion is preferably a silver halide emulsion particularly having a silver chloride content of 98 mol% or more.
- silver halide grains having a silver bromide localized phase on the surface of silver chloride grains are particularly preferable, because a high sensitivity can be obtained and the photographic performance can be stabilized.
- the silver halide emulsion contained in at least one light-sensitive silver halide emulsion layer is preferably a monodisperse emulsion wherein the deviation coefficient of the grain size distribution (obtained by dividing the standard deviation of the grain size distribution by the average grain size) is preferably 15% or less and more preferably 10% or less. Further, for the purpose of obtaining a wide latitude, two or more of such monodisperse emulsions are mixed and are used in the same layer, preferably. In that case, the monodisperse emulsions are different in the average grain size preferably by 15% or more, more preferably 20 to 60%, and further particularly preferably 25 to 50%. Further, the monodisperse emulsions are different in sensitivity preferably by 0.15 to 0.50 log E (log E is the logarithmic exposure amount), more preferably 0.20 to 0.40 log E, and further more preferably 0.25 to 0.35 log E.
- log E is the logarithmic exposure amount
- a silver halide emulsion wherein silver bromochloride, having a silver chloride content of 95 mol% or more and substantially free from silver iodide, contains an iron and/or ruthenium and/or osmium compound in an amount of 1 x 10 -5 to 1 x 10 -3 mol per mol of the silver halide, and wherein a silver bromide localized phase contains an iridium compound in an amount of 1 x 10 -7 to 1 x 10 -5 mol per mol of the silver halide.
- the silver halide emulsion generally one is used that is physically ripened and/or chemically ripened and spectrally sensitized. Additives used in such steps are described in RD Nos. 17643, 18716, and 307105, and the pertinent sections thereof are collected in the table below.
- two or more emulsions different in at least one of the following properties: that are the grain size of the light-sensitive silver halide emulsion, the grain size distribution, the halogen composition, the shape of the grains, and the sensitivity, can be mixed for use in the same layer.
- Silver halide grains whose surfaces are fogged, described in US-A-4 082 553; silver halide grains whose insides are fogged, described in US-A-4 626 498 and JP-A-59-214852; or colloidal silver, is preferably applied in the light-sensitive silver halide emulsion layer and/or the substantially non-light-sensitive hydrophilic colloid layer.
- the term "silver halide grains whose insides or surfaces are fogged” means silver halide grains whose entire exposed part and unexposed part of the light-sensitive material can be subjected to development uniformly (un-imagewise), and the method of preparing them is described in US-A-4 626 498 and JP-A-59-214852.
- the silver halide that forms the inside nuclei of the core/shell-type silver halide grains whose insides are fogged, may be made different in the silver halide composition.
- any of silver chloride, silver bromochloride, silver bromoiodide, and silver bromoiodochloride can be used as the silver halide whose grains' insides or surfaces are fogged.
- the average grain size of these fogged silver halide grains is preferably 0.01 to 0.75 ⁇ m, and particularly preferably 0.05 to 0.6 ⁇ m.
- the shape of the grains may be regular, and the emulsion may be a polydisperse emulsion, but it is preferably a monodisperse emulsion (wherein at least 95% of the number of the silver halide grains or the weight of the silver halide grins falls within grains whose diameters are the average grain diameter ⁇ 40%).
- a transmission-type base or a reflective-type base can be used as the photographic base.
- a transparent film such as a cellulose nitrate film and a polyethylene terephthalate film, and one wherein a film, for example, of a polyester of 2,6-naphthalenedicarboxylic acid (NDCA) with ethylene glycol (EG) or a polyester of NDCA, terephthalic acid, and EG, is provided with an information recording layer, such as a magnetic layer, are preferably used.
- a reflective-type base is preferably used, and particularly preferably a reflective-type base, wherein a laminate has a plurality of polyethylene layers or polyester layers and wherein at least one of such water-resistant resin layers (laminated layers) contains a white pigment, such as titanium oxide, is used.
- the above water-resistant resin layers contain a fluorescent whitening agent.
- a fluorescent whitening agent may be dispersed in the hydrophilic colloid layer of the light-sensitive material.
- a fluorescent whitening agent preferably a benzoxazole-series fluorescent whitening agent, a cumarin-series fluorescent whitening agent, or a pyrazoline-series fluorescent whitening agent can be used, and more preferably a benzoxazolylnaphthalene-series fluorescent whitening agent or a benzoxazolylstilbene-series fluorescent whitening agent is used.
- the amount to be used is not particularly limited, but preferably it is 1 to 100 mg/m 2 .
- the mixing proportion is 0.0005 to 3% by weight, and more preferably 0.001 to 0.5% by weight, to the resin.
- a hydrophilic colloid layer containing a white pigment may be applied on the base.
- the reflective-type base may be a base having a specular reflective or a second-type diffusion reflective metal surface.
- the hydrophilic colloid layer contains a dye that can be decolored by processing (an oxonol dye inter alia), as described in European Patent EP-A-0,337,490(A2), pages 27 to 76, so that the optical reflection density of the light-sensitive material at 680 nm may be 0.70 or more, or preferably the water-resistant resin layer of the base contains 12% by weight or more (more preferably 14% by weight or more) of titanium oxide whose surface has been treated with a bivalent to tetravalent alcohol (e.g. trimethylolethane).
- a bivalent to tetravalent alcohol e.g. trimethylolethane
- a mildewproofing agent as described in JP-A-63-271247 to the light-sensitive material according to the present invention, in order to prevent the proliferation of various mildew and fungus that will otherwise proliferate in the hydrophilic colloid layer to deteriorate images.
- the light-sensitive material according to the present invention may be exposed to visible light or infrared radiation.
- the method of exposure may be of low-intensity exposure or high-intensity short-period exposure, and particularly, in the latter case, a laser scanning exposure system is preferable, wherein the exposure time per pixel is shorter than 10 -4 sec.
- the present invention when the above pyrrolotriazole-type coupler is contained, the effect of the present invention in improving the whiteness of the white background is great, but the method of the present invention can be applied also to light-sensitive materials containing another cyan coupler besides the above coupler.
- the cyan coupler, the magenta coupler, or the yellow coupler is impregnated into a loadable latex polymer (e.g. US-A-4 203 716) in the presence (or absence) of a high-boiling organic solvent shown in the above table, or the coupler is dissolved together with a water-insoluble and organic-solvent-soluble polymer, and the resulting solution is emulsified and dispersed in an aqueous hydrophilic colloid solution.
- a loadable latex polymer e.g. US-A-4 203 716
- the coupler is dissolved together with a water-insoluble and organic-solvent-soluble polymer, and the resulting solution is emulsified and dispersed in an aqueous hydrophilic colloid solution.
- Preferable water-insoluble and organic-solvent-soluble polymers are homopolymers or copolymers described in US-A-4 857 449, columns 7 to 15, and International Publication WO 88/00723, pages 12 to 30.
- methacrylate polymers and acrylamide polymers are particularly preferable, in view of image dye stability and the like.
- a dye-image-preservability-improving compound as described in European Patent EP-A-0,277,589(A2) is used in combination with a pyrazoloazole coupler, the above pyrrolotriazole coupler, or an acylacetamide-type yellow coupler.
- cyan couplers in addition to phenol-type couplers and naphthol-type couplers as described in the known documents in the above table, cyan couplers, as described in JP-A-2-33144, European Patent EP-A-0,333,185(A2), JP-A-64-32260, European Patent EP-A-0,456,226(A1), European Patent EP-A-0,484,909, European Patent EP-A-0,488,248, and EP-A-0,491,197(A1), can be used.
- magenta coupler used in the present invention in addition to 5-pyrazolone-series magenta couplers as described in the known documents in the above table, those described in International Publication WO 92/18901, WO 92/18902, and WO 92/18903 are also preferable.
- pyrazoloazole-type couplers can be used in the present invention, and among them, pyrazoloazoles described in JP-A-61-65245, JP-A-61-65246, JP-A-61-14254, and European Patents EP-A-226,849, and EP-A-294,785 are preferably used in view of the hue, the image stability, the color-forming property, and the like.
- acylacetanilide-type couplers are preferably used, and among them, couplers described in European Patent EP-A-0,447,969, JP-A-5-107701, JP-A-5-113642, European Patent EP-A-0,482,552, and EP-A-0,524,540 are preferably used.
- Couplers for correcting undesired absorption of color-formed dyes are preferably yellow-colored cyan couplers represented by formula (CI), (CII), (CIII), or (CIV) (particularly YC-86 on page 84) described in EP-A-456,257(A1), page 5; yellow-colored magenta couplers ExM-7 (page 202), EX-1 (page 249), and EX-7 (page 251) described in EP-A-456,257(A1); magenta-colored cyan couplers CC-9 (column 8) and CC-13 (column 10) described in US-A-4 833 069; (2) (column 8) of US-A-4 837 136, and colorless masking couplers (particularly, exemp
- the processing method of the silver halide color photographic light-sensitive material of the present invention even when a processing solution is regenerated repeatedly with the used amount of its regenerating agent lessened, to recycle it, such excellent effects can be attained that no stain occurs, that good bleaching can be effected, and that the load on the environment can be decreased.
- Layers having the below-shown compositions were formed on a cellulose triacetate film support (base), that had been provided an undercoat, to prepare a multi-layer color photographic light-sensitive material.
- Figures corresponding to each component represents the coating amount in terms of g/m 2 , and for silver halide in terms of silver. With respect to sensitizing dyes, the coating amount is shown in mol, per mol of silver halide in the same layer.
- Silver bromoiodide emulsion M silver 0.065 ExC-2 0.04 Polyethyl acrylate latex 0.20 Gelatin 1.04
- Silver bromoiodide emulsion A silver 0.25 Silver bromoiodide emulsion B silver 0.25 ExS-1 6.9 x 10 -5 ExS-2 1.8 x 10 -5 ExS-3 3.1 x 10 -4 ExC-1 0.17 ExC-3 0.030 ExC-4 0.10 ExC-5 0.020 ExC-6 0.010 Cpd-2 0.025 HBS-1 0.10 Gelatin 0.87
- Silver bromoiodide emulsion D silver 1.40 ExS-1 2.4 x 10 -4 ExS-2 1.0 x 10 -4 ExS-3 3.4 x 10 -4 ExC-1 0.10 ExC-3 0.045 ExC-6 0.020 ExC-7 0.010 Cpd-2 0.050 HBS-1 0.22 HBS-2 0.050 Gelatin 1.10
- Silver bromoiodide emulsion E silver 0.15 Silver bromoiodide emulsion F silver 0.10 Silver bromoiodide emulsion G silver 0.10 ExS-4 3.0 x 10 -5 ExS-5 2.1 x 10 -4 ExS-6 8.0 x 10 -4 ExM-2 0.33 ExM-3 0.086 ExY-1 0.015 HBS-1 0.30 HBS-3 0.010 Gelatin 0.73
- Silver bromoiodide emulsion I silver 1.25 ExS-4 3.7 x 10 -5 ExS-5 8.1 x 10 -5 ExS-6 3.2 x 10 -4 ExC-1 0.010 ExM-1 0.020 ExM-4 0.025 ExM-5 0.040 Cpd-3 0.040 HBS-1 0.25 Polyethyl acrylate latex 0.15 Gelatin 1.33
- Silver bromoiodide emulsion L silver 1.00 ExS-7 4.0 x 10 -4 ExY-2 0.10 ExY-3 0.10 ExY-4 0.010 Cpd-2 0.10 Cpd-3 1.0 x 10 -3 HBS-1 0.070 Gelatin 0.70
- UV-1 0.19 UV-2 0.075 UV-3 0.065 HBS-1 5.0 x 10 -2 HBS-4 5.0 x 10 -2 Gelatin 1.8
- Silver bromoiodide emulsion M silver 0.10 H-1 0.40 B-1 (diameter: 1.7 ⁇ m) 5.0 x 10 -2 B-2 (diameter: 1.7 ⁇ m) 0.15 B-3 0.05 S-1 0.20 Gelatin 70
- compounds of W-1 to W-3, B-4 to B-6, and F-1 to F-17, and salts of iron, lead, gold, platinum, palladium, iridium, and rhodium were suitably added in each layer.
- the content was recovered, and added into 8 g of 12.5% aqueous gelatin solution. Then the beads were removed by filtration, and a gelatin dispersion of the dye was obtained. The average grain diameter of the fine grains of the dye was 0.44 ⁇ m.
- Dispersions of ExF-3, ExF-4, and ExF-6 in the form of solid fine grains were obtained in the same manner as above. Average grain diameters of the fine grains of the dye were 0.24 ⁇ m, 0.45 ⁇ m and 0.52 ⁇ m, respectively.
- ExF-5 was dispersed by the microprecipitation dispersion method as described in Example 1 of EP-A-549,489. The average grain diameter of the fine grains of ExF-5 was 0.06 ⁇ m.
- Sample 101 was exposed to light imagewise and was continuously processed with processing solutions that were prescribed as shown below, until the cumulative total of the replenishment rate of the bleaching solution reached 8,000 ml.
- the overflow was regenerated every 100 liters.
- the regeneration was carried out in such a manner that a bleaching replenisher 2, from a replenishing tank 1, was supplied to a bleaching solution 3, in a bleaching tank 4, and the overflow 6 from the bleaching bath 4 was stored in a stock tank 5. Every time the overflow accumulated in an amount of 100 liters, air 8 was blown through the stored overflow 6 by an air pump 7, for 4 hours.
- the below-described bleaching-solution-regenerating agent 13 was added in the amount shown in Table 3, to prepare a regenerated replenisher, and the regenerated replenisher was used as a bleaching replenisher from the next time, to continue the processing.
- 9 is a pipe of air from the air pump 7 to an air-blowing part 10 in the stock tank 5; 11 is a stirrer; and 12 is a pipe of the regenerated replenisher to the replenishing tank.
- processing step Processing Replenishing rate Tank Volume /liter time temperature Color-developing 3 min 15 sec 38.0 °C 630 ml 2 Bleaching 3 min 00 sec 38.0 °C 715 ml 2 Washing (1) 30 sec 38.0 °C 430 ml 2 Fixing 3 min 00 sec 38.0 °C 430 ml 2 Washing (2) 1 min 00 sec 38.0 °C 770 ml 2 Stabilizing 30 sec 38.0 °C 570 ml 2 Drying 3 min 50.0 °C - -
- Washing (1) was separated to 2 tanks, and washing (2) was separated to 3 tanks, and each washing was carried out in a counter current mode from back side to forward. Further, in each step, the carried over amount of tank solution to the next step were respectively 60 ml, per m 2 of the light-sensitive material. Each crossover time was 3 sec which was included in the processing time of the preceding step.
- composition of each processing solution was as follows, respectively:
- Bleaching agent shown in Table 2 Maleic acid 33 g Succinic acid 36 g Ammonium nitrate 7 g Potassium bromide 60 g Water to make 1.0 liter pH (pH was adjusted by aqueous ammonia) 4.9
- the start replenisher was diluted to 1.1 times, and pH was adjusted to 5.0 with aqueous ammonia, to use as a start tank solution.
- Bleaching agent shown in Table 2 Maleic acid 56 g Succinic acid 60 g Ammonium nitrate 14 g Potassium bromide 80 g Water to make 1.0 liter pH (pH was adjusted by aqueous ammonia) 3.8
- Tap water was treated by passage through a mixed bed ion-exchange column filled with H-type strong acidic cation exchange resin (Amberlite IR-120B, trade name, made by Rohm & Haas) and OH-type strong basic anion exchange resin (Amberlite IRA-400, the same as the above) so that the concentrations of Ca ions and Mg ions in water were both made to decrease to 3 mg/liter or below, followed by adding 20 mg/liter of sodium dichlorinated isocyanurate and 150 mg/liter of sodium sulfate. The pH of this water was in the range of 6.5 to 7.5.
- H-type strong acidic cation exchange resin Amberlite IR-120B, trade name, made by Rohm & Haas
- Amberlite IRA-400 OH-type strong basic anion exchange resin
- Dmin yellow transmission density
- the support and the backing layer of the light-sensitive material were prepared as described below, and the light-sensitive layers as described in the above Example 1 were coated on the support, to prepare a light-sensitive material Sample 102.
- the support that was used in this example was prepared as follows:
- a blue dye, a magenta dye, and a yellow dye (I-1, I-4, I-6, I-24, I-26, I-27, II-5, as described in Kokai Giho: Kogi No. 94-6023) were added. Further, this film was wound around a stainless steel core (spool) having a diameter of 20 cm, and thermal history was imparted thereto at 110 °C for 48 hours, to obtain a support having suppressed core-set-curl.
- the undercoat layer was provided on the side that was heated at a higher temperature at the time of stretching. Drying was carried out at 115 °C for 6 minutes (the roller and the transportation apparatus in the drying zone all were set at 115 °C).
- Silica grains (0.3 ⁇ m), as a matting agent, and 3-poly(polymerization degree: 15) oxyethylene-propyloxytrimethoxysilan (15 weight%)-coated aluminum oxide (0.15 ⁇ m), as an abrasive, were each added thereto, to give a coverage of 10 mg/m 2 . Drying was conducted at 115 °C for 6 min (the roller and the transportation apparatus in the drying zone all were set at 115 °C). The increment of the color density of D B of the magnetic recording layer was about 0.1 when X-light (blue filter) was used. The saturation magnetization moment of the magnetic recording layer was 4.2 emu/g, the coercive force was 7.3 x 10 4 A/m, and the squareness ratio was 65%.
- Diacetyl cellulose (25 mg/m 2 ), and a mixture of C 6 H 13 CH(OH)C 10 H 20 COOC 40 H 81 (Compound a, 6 mg/m 2 ) and C 50 H 101 O(CH 2 CH 2 O) 16 H (Compound b, 9 mg/m 2 ) was coated.
- the mixture was dissolved in a solution of xylene and propyleneglycol monomethylether (1/1) at 105 °C, and this solution was poured into a 10-fold volume of propyleneglycol monomethylether (normal temperature) and finely dispersed. This was further dispersed in acetone, and the obtained dispersion (average grain diameter: 0.01 ⁇ m) was added to the coating solution.
- Silica grains (0.3 ⁇ m), as a matting agent, and 3-poly(polymerization degree, 15) oxyethylene-propyloxytrimethoxysilan (15 weight%)-coated aluminum oxide (0.15 ⁇ m), as an abrasive, were each added thereto, to give a coverage of 15 mg/m 2 .
- the slipping layer was dried at 115 °C for 6 minutes (the roller and the transportation apparatus in the drying zone all were set at 115 °C).
- the slipping layer showed excellent performances of the coefficient of dynamic friction: 0.06 (a stainless steel hard ball of 5 mm ⁇ , diameter, load: 100 g, speed: 6 cm/min), and of the static friction coefficient: 0.07 (clip method).
- the sliding property of the slipping layer with the surface of the emulsion which will be described below, was also excellent, such that the coefficient of dynamic friction was 0.12.
- the thus-prepared Sample 102 was cut into a strip having a length of 160 cm and a width of 24 mm. Two perforations of 2 mm square were made at intervals of 5.8 mm, located at the position of 0.7 mm in the width direction and at one side in the lengthwise direction of the light-sensitive material, respectively. Further, sets of such two perforations were made at intervals of 32 mm.
- the sample was encased in a plastic film cartridge, as illustrated in Fig. 1 to Fig. 7 of US-A-5,296,887.
- the sample 102 was set in a camera with a built-in magnetic recording device having a headgap of 5 ⁇ m, a turn number of 50, and made of permalloy. A digital saturation recording using a recording wavelength of 50 ⁇ m and photographing were conducted with the camera.
- Tte thus-photographed Sample 102 was continuously processed with processing solutions and processing methods as shown below until the cumulative total of the replenishment rate of the bleaching solution reached 6,000 ml.
- the overflow was regenerated every 1 liter.
- the regeneration was carried out in such a manner that a bleaching replenisher 2, from a replenishing tank 1, was supplied to a bleaching solution 3, in a bleaching tank 4, and the overflow 6 from the bleaching tank 4 was stored in a stock tank 5. Every time the overflow accumulated in an amount of 1 liter, air 8 was blown through the stored overflow 6 by an air pump 7, for 4 hours. Thereafter, 50 ml of the below-described bleaching-solution-regenerating agent 13 was added, to prepare a regenerated replenisher, and the regenerated replenisher was used as a bleaching replenisher from the next time, to continue the processing.
- Washing (1) was separated to 2 tanks, and washing (2) was separated to 3 tanks, and each washing was carried out in a counter current mode from back side to forward. Further, in each step, the carried over amount of tank solution to the next step were respectively 60 ml, per m 2 of the light-sensitive material. Each crossover time was 3 sec which was included in the processing time of the preceding step.
- composition of each processing solution was as follows, respectively:
- the color-developer, the fixing solution, and the washing water used were the same as those in the above Example 1, for both the mother solution and the replenisher.
- Dmin yellow transmission density
- Example 1 The experiments of Example 1 were carried out in the same manner as in Example 1, except that a Developing Apparatus FNCP900II, manufactured by Fuji Photo Film Co., Ltd., was used.
- a Developing Apparatus FNCP900II manufactured by Fuji Photo Film Co., Ltd.
- another level of experiment was carried out in this Example. That is, in the another level of experiment, the added amount of the bleaching-solution-regenerating agent per 100 liters of the overflow was further reduced to 4 liters, which meant that the regenerating agent was used in an amount of 28.6 ml per square meter of the processed light-sensitive material.
- Example 2 The experiments of Example 2 were conducted using a Developing Apparatus FNCP900II, manufactured by Fuji Photo Film Co., Ltd. This example was conducted in the same manner as in Example 2, except that the added amount of the bleaching-solution-regenerating agent was reduced from 50 ml to 39 ml, per liter of the overflow. As a result, results almost the same as those of Example 2 were attained.
- the coating solutions for each photographic constitutional layer were prepared as follows.
- the below shown "average grain size of emulsion" means an average value of an estimate diameter calculated from the area of grains measured with a so-called projection-area method.
- a cyan coupler (the below-shown acylaminophenol coupler (Sample A) or pyrrolotriazole coupler (Sample B) was used, respectively), 250 g of a color-image-stabilizer (Cpd-1), 10 g of a color-image-stabilizer (Cpd-9), 10 g of a color-image-stabilizer (Cpd-10), 20 g of a color-image-stabilizer (Cpd-12), 14 g of an ultraviolet absorbing agent (UV-1), 50 g of an ultraviolet absorbing agent (UV-2), 40 g of an ultraviolet absorbing agent (UV-3), and 60 g of an ultraviolet absorbing agent (UV-4) were dissolved in 230 g of a solvent (Solv-6) and 350 ml of ethyl acetate, and the resulting solution was emulsified and dispersed in 6500 g of a 10% aqueous gelatin solution containing 200 ml of 10% sodium dodecylbenz
- a silver chlorobromide emulsion C (cubes, a mixture of a large-size emulsion C having an average grain size of 0.50 ⁇ m, and a small-size emulsion C having an average grain size of 0.41 ⁇ m (1 : 4 in terms of mol of silver), the deviation coefficients of the grain size distributions being 0.09 and 0.11 respectively, and each emulsion having 0.5 mol % of silver bromide locally contained in part of the grain surface whose substrate was made up of silver chloride) was prepared.
- the above emulsified dispersion C and this silver chlorobromide emulsion C were mixed and dissolved, and a fifth-layer coating solution was prepared so that it would have the composition shown below.
- the coating amount of the emulsion is in terms of silver.
- the coating solutions for the first layer to forth layer and the sixth layer to seventh layer were prepared in the similar manner as that for the fifth layer coating solution.
- As the gelatin hardener for each layer 1-oxy-3,5-dichloro-s-triazine sodium salt was used.
- the sensitizing dyes A, B, and C were added, respectively, to the large-size emulsion, in an amount of 1.4 x 10 -4 mol per mol of the silver halide, and to the small-size emulsion in an amount of 1.7 x 10 -4 per mol of the silver halide.
- the sensitizing dye D was added to the large-size emulsion in an amount of 3.0 x 10 -4 mol per mol of the silver halide, and to the small-size emulsion in an amount of 3.6 x 10 -4 mol per mol of the silver halide;
- the sensitizing dye E was added to the large-size emulsion in an amount of 4.0 x 10 -5 mol per mol of the silver halide, and to the small-size emulsion in an amount of 7.0 x 10 -5 mol per mol of the silver halide;
- the sensitizing dye F was added to the large-size emulsion in an amount of 2.0 x 10 -4 mol per mol of the silver halide, and to the small-size emulsion in an amount of 2.8 x 10 -4 mol per mol of the silver halide.
- the sensitizing dyes G and H were added, respectively, to the large-size emulsion, in an amount of 6.0 x 10 -5 mol per mol of the silver halide, and to the small-size emulsion in an amount of 9.0 x 10 -5 per mol of the silver halide.
- the following compound I was added in the red-sensitive emulsion layer in an amount of 2.6 x 10 -3 mol per mol of the silver halide.
- the fourth layer was added in amounts of 0.2 mg/m 2 , 0.2 mg/m 2 , 0.6 mg/m 2 , and 0.1 mg/m 2 , respectively.
- disodium catechol-3,5-disulfonate in amounts of 6 mg/m 2 , 6 mg/m 2 , and 18 mg/m 2 , respectively.
- the following dyes were added to the emulsion layers (the coating amount is shown in parentheses).
- each layer is shown below.
- the numbers show coating amounts (g/m 2 ).
- the coating amount is in terms of silver.
- Polyethylene resin-Laminated Paper [The polyethylene resin on the first layer side contained a white pigment (TiO 2 : content of 16 wt%, ZnO: content of 4 wt%), a fluorescent whitening agent (4,4-bis(5-methylbenzoxazoryl)stilbene: content of 0.05 wt%), and a blue dye (ultramarine)]
- a white pigment TiO 2 : content of 16 wt%, ZnO: content of 4 wt%)
- a fluorescent whitening agent (4,4-bis(5-methylbenzoxazoryl)stilbene: content of 0.05 wt%)
- blue dye (ultramarine)
- a silver chlorobromide emulsion cubes, a mixture of a large-size emulsion A having an average grain size of 0.72 ⁇ m, and a small-size emulsion A having an average grain size of 0.60 ⁇ m (3 : 7 in terms of mol of silver).
- the deviation coefficients of the grain size distributions were 0.08 and 0.10, respectively, and each emulsion had 0.3 mol % of AgBr locally contained in part of the grain surface whose substrate was made up of silver chloride.
- Second Layer Color-Mixing Inhibiting Layer
- a silver chlorobromide emulsion B cubes, a mixture of a large-size emulsion B having an average grain size of 0.45 ⁇ m, and a small-size emulsion B having an average grain size of 0.35 ⁇ m (1 : 3 in terms of mol of silver).
- the deviation coefficients of the grain size distributions were 0.10 and 0.08, respectively, and each emulsion had 0.4 mol % of AgBr locally contained in part of the grain surface whose substrate was made up of silver chloride.
- a silver chlorobromide emulsion C cubes, a mixture of a large-size emulsion C having an average grain size of 0.50 ⁇ m, and a small-size emulsion C having an average grain size of 0.41 ⁇ m (1 : 4 in terms of mol of silver).
- the deviation coefficients of the grain size distributions were 0.09 and 0.11, respectively, and each emulsion had 0.5 mol % of silver bromide locally contained in part of the grain surface whose substrate was made up of silver chloride.
- Cyan coupler (A or B) 0.30 Ultraviolet absorbing agent (UV-1) 0.14 Ultraviolet absorbing agent (UV-2) 0.05 Ultraviolet absorbing agent (UV-3) 0.04 Ultraviolet absorbing agent (UV-4) 0.06 Color-image stabilizer (Cpd-1) 0.25 Color-image stabilizer (Cpd-9) 0.01 Color-image stabilizer (Cpd-10) 0.01 Color-image stabilizer (Cpd-12) 0.02 Solvent (Solv-6) 0.23
- UV-1 0.19 Ultraviolet absorbing agent
- UV-2 0.06 Ultraviolet absorbing agent
- UV-3 0.06 Ultraviolet absorbing agent
- UV-4 0.05 Ultraviolet absorbing agent
- UV-5) 0.09
- Solvent (Solv-7) 0.25
- the thus-prepared color photographic light-sensitive material was formed into a roll with a width of 127 mm, it was exposed to light imagewise by an automatic printer, and it was processed using an automatic processor in the way described below, until the accumulative total of the replenishing rate of the bleaching solution reached 3 times the tank volume of the bleaching solution.
- the overflow was regenerated every 10 liters.
- the regeneration was carried out in the same way as in Example 1, and the blowing of air at the regeneration was carried out for 2 hours.
- the regenerating agent used therein is shown below.
- the amount carried over from the preceding bath by the light-sensitive material was 80 ml.
- composition of each processing solution was as follows, respectively:
- Dimethylpolysiloxane-series surface active agent (Silicone KF351A, trade name: manufactured by Shinetsu Kagaku Kogyo Co.) 0.1 g 0.1 g Triisopropanolamine 15.0 g 15.0 g Ethylenediaminetetraacetic acid 4.0 g 4.0 g Sodium 4,5-dihydroxybenzene -1,3-disulfonate 0.5 g 0.5 g Potassium chloride 10.0 g - Potassium bromide 0.04 g 0.01 g Fluorescent whitening agent (Blankophor BSU-PN, trade name: manufactured by Bayer AG) 5.0 g 15.0 g Fluorescent whitening agent (Hakkol BRK, trade name: manufactured by Showa Kagaku Co.) 0.5 g 2.0 g Sodium sulfite 0.1 g 0.1 g Disodium-N,N-bis(s) 0.5 g 2.0 g Sodium sulfite
- the start bleaching replenisher was prepared by diluting the bleaching-regenerating agent shown below 4 times, and its pH was adjusted to 3.2 by 20% sulfuric acid.
- the below-shown bleaching-regenerating agent was diluted 6 times, and its pH was adjusted to 3.4 in the same manner as in the replenisher.
- Bleaching agent (described in Table 7, the ferric complex salt of each compound was used) 1,3-Diaminopropanetetraacetic acid 63 g 25% Aqueous ammonia 30 g 70% Glycolic acid 20 g 75% Acetic acid 60 g Ferric nitrate ⁇ nonahydrate 167 g Ammonium bromide 110 g Water to make 1.0 liter pH (pH was adjusted by using aqueous ammonia) 3.2 No Start bleaching replenisher Bleaching-regenerating agent 1 I - 15 27 g 52 g 2 1,3-diaminopropanetetraacetic acid 34 g 59 g 3 Ethylenediamine-N,N'-disuccinic acid 33 g 58 g
Landscapes
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Silver Salt Photography Or Processing Solution Therefor (AREA)
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP10243597 | 1997-04-07 | ||
JP10243597 | 1997-04-07 | ||
JP102435/97 | 1997-04-07 |
Publications (2)
Publication Number | Publication Date |
---|---|
EP0871065A1 true EP0871065A1 (de) | 1998-10-14 |
EP0871065B1 EP0871065B1 (de) | 2002-08-28 |
Family
ID=14327398
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP98106286A Expired - Lifetime EP0871065B1 (de) | 1997-04-07 | 1998-04-06 | Verarbeitungsverfahren für ein lichtempfindliches, photographisches Silberhalogenidfarbmaterial |
Country Status (3)
Country | Link |
---|---|
EP (1) | EP0871065B1 (de) |
AT (1) | ATE223075T1 (de) |
DE (1) | DE69807383T2 (de) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP0996035A1 (de) * | 1998-10-20 | 2000-04-26 | Eastman Kodak Company | Ein Verfahren zur schnellen photographischen Verarbeitung |
US7160674B2 (en) | 2003-08-29 | 2007-01-09 | A&O Imagining Solutions Gmbh | Photographic chemicals bundle |
Citations (8)
Publication number | Priority date | Publication date | Assignee | Title |
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EP0329088A2 (de) * | 1988-02-15 | 1989-08-23 | Konica Corporation | Verfahren zur Verarbeitung und Bleichlösung für farbphotographische lichtempfindliche Silberhalogenidmaterialien |
US4923785A (en) * | 1987-07-15 | 1990-05-08 | Agfa Gevaert Ag | Bleaching bath concentrate |
JPH03134664A (ja) * | 1989-10-20 | 1991-06-07 | Fuji Photo Film Co Ltd | ハロゲン化銀写真感光材料の処理方法 |
EP0488233A1 (de) * | 1990-11-27 | 1992-06-03 | Fuji Photo Film Co., Ltd. | Verfahren zur Verarbeitung eines photographischen Silberhalogenidmaterials |
US5153111A (en) * | 1990-01-24 | 1992-10-06 | Fuji Photo Film Co., Ltd. | Composition for color-development and method for processing using same |
EP0512318A2 (de) * | 1991-05-04 | 1992-11-11 | Agfa-Gevaert AG | Fotografisches Verarbeitungsverfahren |
JPH086220A (ja) * | 1994-06-17 | 1996-01-12 | Fuji Photo Film Co Ltd | ハロゲン化銀カラー写真感光材料の処理方法及びそれに用いられる漂白液再生剤 |
US5580705A (en) * | 1991-12-27 | 1996-12-03 | Konica Corporation | Method of bleaching silver halide color photographic light-sensitive materials using particular ferric chelates |
-
1998
- 1998-04-06 AT AT98106286T patent/ATE223075T1/de not_active IP Right Cessation
- 1998-04-06 EP EP98106286A patent/EP0871065B1/de not_active Expired - Lifetime
- 1998-04-06 DE DE69807383T patent/DE69807383T2/de not_active Expired - Lifetime
Patent Citations (8)
Publication number | Priority date | Publication date | Assignee | Title |
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US4923785A (en) * | 1987-07-15 | 1990-05-08 | Agfa Gevaert Ag | Bleaching bath concentrate |
EP0329088A2 (de) * | 1988-02-15 | 1989-08-23 | Konica Corporation | Verfahren zur Verarbeitung und Bleichlösung für farbphotographische lichtempfindliche Silberhalogenidmaterialien |
JPH03134664A (ja) * | 1989-10-20 | 1991-06-07 | Fuji Photo Film Co Ltd | ハロゲン化銀写真感光材料の処理方法 |
US5153111A (en) * | 1990-01-24 | 1992-10-06 | Fuji Photo Film Co., Ltd. | Composition for color-development and method for processing using same |
EP0488233A1 (de) * | 1990-11-27 | 1992-06-03 | Fuji Photo Film Co., Ltd. | Verfahren zur Verarbeitung eines photographischen Silberhalogenidmaterials |
EP0512318A2 (de) * | 1991-05-04 | 1992-11-11 | Agfa-Gevaert AG | Fotografisches Verarbeitungsverfahren |
US5580705A (en) * | 1991-12-27 | 1996-12-03 | Konica Corporation | Method of bleaching silver halide color photographic light-sensitive materials using particular ferric chelates |
JPH086220A (ja) * | 1994-06-17 | 1996-01-12 | Fuji Photo Film Co Ltd | ハロゲン化銀カラー写真感光材料の処理方法及びそれに用いられる漂白液再生剤 |
Non-Patent Citations (3)
Title |
---|
COOLEY A ET AL: "FACTORS LIMITING THE RECOVERY, REGENERATION, AND REUSE OF PHOTOGRAPHIC PROCESSING SOLUTIONS", JOURNAL OF IMAGING SCIENCE AND TECHNOLOGY, vol. 37, no. 6, 1 November 1993 (1993-11-01), pages 603 - 606, XP000422491 * |
PATENT ABSTRACTS OF JAPAN vol. 015, no. 352 (P - 1248) 6 September 1991 (1991-09-06) * |
PATENT ABSTRACTS OF JAPAN vol. 096, no. 005 31 May 1996 (1996-05-31) * |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP0996035A1 (de) * | 1998-10-20 | 2000-04-26 | Eastman Kodak Company | Ein Verfahren zur schnellen photographischen Verarbeitung |
US6174653B1 (en) | 1998-10-20 | 2001-01-16 | Eastman Kodak Company | Method for rapid photographic processing |
US7160674B2 (en) | 2003-08-29 | 2007-01-09 | A&O Imagining Solutions Gmbh | Photographic chemicals bundle |
Also Published As
Publication number | Publication date |
---|---|
ATE223075T1 (de) | 2002-09-15 |
EP0871065B1 (de) | 2002-08-28 |
DE69807383T2 (de) | 2003-01-09 |
DE69807383D1 (de) | 2002-10-02 |
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