EP0486909A1 - Fixierbad - Google Patents
Fixierbad Download PDFInfo
- Publication number
- EP0486909A1 EP0486909A1 EP91119130A EP91119130A EP0486909A1 EP 0486909 A1 EP0486909 A1 EP 0486909A1 EP 91119130 A EP91119130 A EP 91119130A EP 91119130 A EP91119130 A EP 91119130A EP 0486909 A1 EP0486909 A1 EP 0486909A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- alkyl
- hydroxy
- ammonium
- carboxy
- fixing
- 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
- 239000008139 complexing agent Substances 0.000 claims abstract description 12
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 4
- 229910052739 hydrogen Inorganic materials 0.000 claims description 4
- 239000001257 hydrogen Substances 0.000 claims description 4
- 239000011734 sodium Substances 0.000 claims description 4
- 229910052708 sodium Inorganic materials 0.000 claims description 4
- 125000000008 (C1-C10) alkyl group Chemical group 0.000 claims description 3
- ILROLYQPRYHHFG-UHFFFAOYSA-N 1-$l^{1}-oxidanylprop-2-en-1-one Chemical group [O]C(=O)C=C ILROLYQPRYHHFG-UHFFFAOYSA-N 0.000 claims description 3
- 125000004066 1-hydroxyethyl group Chemical group [H]OC([H])([*])C([H])([H])[H] 0.000 claims description 3
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 3
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 3
- 229910052744 lithium Inorganic materials 0.000 claims description 3
- 239000011591 potassium Substances 0.000 claims description 2
- 229910052700 potassium Inorganic materials 0.000 claims description 2
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims 2
- 239000013543 active substance Substances 0.000 claims 1
- 150000001875 compounds Chemical class 0.000 claims 1
- 239000000126 substance Substances 0.000 claims 1
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 7
- -1 silver halide Chemical class 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 229910052709 silver Inorganic materials 0.000 description 4
- 239000004332 silver Substances 0.000 description 4
- 229910001424 calcium ion Inorganic materials 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 description 2
- KEAYESYHFKHZAL-UHFFFAOYSA-N Sodium Chemical compound [Na] KEAYESYHFKHZAL-UHFFFAOYSA-N 0.000 description 2
- XYXNTHIYBIDHGM-UHFFFAOYSA-N ammonium thiosulfate Chemical compound [NH4+].[NH4+].[O-]S([O-])(=O)=S XYXNTHIYBIDHGM-UHFFFAOYSA-N 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 229910001425 magnesium ion Inorganic materials 0.000 description 2
- MGFYIUFZLHCRTH-UHFFFAOYSA-N nitrilotriacetic acid Chemical compound OC(=O)CN(CC(O)=O)CC(O)=O MGFYIUFZLHCRTH-UHFFFAOYSA-N 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000003672 processing method Methods 0.000 description 2
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 description 2
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 description 2
- 235000019345 sodium thiosulphate Nutrition 0.000 description 2
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 1
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 1
- 229920002284 Cellulose triacetate Polymers 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- NNLVGZFZQQXQNW-ADJNRHBOSA-N [(2r,3r,4s,5r,6s)-4,5-diacetyloxy-3-[(2s,3r,4s,5r,6r)-3,4,5-triacetyloxy-6-(acetyloxymethyl)oxan-2-yl]oxy-6-[(2r,3r,4s,5r,6s)-4,5,6-triacetyloxy-2-(acetyloxymethyl)oxan-3-yl]oxyoxan-2-yl]methyl acetate Chemical compound O([C@@H]1O[C@@H]([C@H]([C@H](OC(C)=O)[C@H]1OC(C)=O)O[C@H]1[C@@H]([C@@H](OC(C)=O)[C@H](OC(C)=O)[C@@H](COC(C)=O)O1)OC(C)=O)COC(=O)C)[C@@H]1[C@@H](COC(C)=O)O[C@@H](OC(C)=O)[C@H](OC(C)=O)[C@H]1OC(C)=O NNLVGZFZQQXQNW-ADJNRHBOSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000011814 protection agent Substances 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 235000010265 sodium sulphite Nutrition 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
-
- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03C—PHOTOSENSITIVE MATERIALS FOR PHOTOGRAPHIC PURPOSES; PHOTOGRAPHIC PROCESSES, e.g. CINE, X-RAY, COLOUR, STEREO-PHOTOGRAPHIC PROCESSES; AUXILIARY PROCESSES IN PHOTOGRAPHY
- G03C5/00—Photographic processes or agents therefor; Regeneration of such processing agents
- G03C5/26—Processes using silver-salt-containing photosensitive materials or agents therefor
- G03C5/38—Fixing; Developing-fixing; Hardening-fixing
Definitions
- the invention relates to a fixing bath which is suitable for processing photographic silver halide materials and which contains a biodegradable limescale inhibitor.
- Ammonium thiosulfate is mainly used for fixing.
- fixer baths whose pH is in the slightly acidic to weakly alkaline range, are usually provided with ethylenediaminetetraacetic acid (EDTA) as a limescale protection agent.
- EDTA ethylenediaminetetraacetic acid
- NTA nitrilotriacetic acid
- the invention has for its object to develop a fixing bath that is free of ammonium ions and EDTA, but has the necessary fixing speed and does not cause deposits.
- the complexing agents are usually used in a concentration of 0.5 to 100 mmol / l, the invention in a preferred form containing 2 to 30 mmol / l of complexing agents.
- the unexpected and surprising effect of the invention lies in the fact that the group of degradable complexing agents according to the invention does not form any precipitation with the calcium and magnesium ions of the preparation water in ammonium-free fixing baths.
- Other degradable complexing agents e.g. NTA, result in solid precipitations after just a few days of standing.
- the fixing bath according to the invention is particularly suitable for color photographic silver halide recording materials which, on a reflective or transparent support (for example paper coated on both sides with polyethylene or cellulose triacetate film), have at least one blue-sensitive, at least one green-sensitive and at least one red-sensitive silver halide emulsion layer, to which at least one yellow coupler, in the order given a purple coupler and at least one cyan coupler are included.
- a reflective or transparent support for example paper coated on both sides with polyethylene or cellulose triacetate film
- the fixing bath according to the invention is used within the usual processing method for silver halide photographic materials.
- the processing method can be carried out continuously with constant regeneration of the individual processing baths.
- the fixing baths listed in the examples are comparable in their fixing behavior to a conventional fixing bath containing EDTA.
- Fixing bath Water (deionized) 800 ml Sodium sulfate 10g Sodium sulfite 20 g Sodium thiosulfate 60 g Calcium chloride solution (80 g / l) 5 ml Complexing agent See table 1 Adjust pH to 8 and make up to 1 liter with deionized water.
Landscapes
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Silver Salt Photography Or Processing Solution Therefor (AREA)
Abstract
Die Erfindung betrifft ein ammoniumfreies Fixierbad, das biologisch gut abbaubar ist und einen Komplexbildner der Formel <IMAGE> enthält, wobei R und M die in der Beschreibung angegebene Bedeutung haben.
Description
- Die Erfindung betrifft ein für die Verarbeitung fotografischer Silberhalogenidmaterialien geeignetes Fixierbad, das ein biologisch abbaubares Kalkschutzmittel enthält.
- Zum Fixieren wird überwiegend Ammoniumthiosulfat verwendet. Diese Fixierbäder, deren pH-Wert im schwach sauren bis schwach alkalischen Bereich liegt, werden üblicherweise mit Ethylendiamintetraessigsäure (EDTA) als Kalkschutzmittel versehen.
- Sowohl Ammoniumionen als auch EDTA werden in ihrem Umweltverhalten als bedenklich eingestuft. Besonders EDTA reichert sich in Abwässern an, da es biologisch nur sehr langsam abgebaut wird. Ersetzt man nun EDTA durch Nitrilotriessigsäure (NTA), deren gute biologische Abbaubarkeit bekannt ist, so bildet sich in einem Fixierbad, das anstelle von Ammoniumthiosulfat das umweltverträglichere Natriumthiosulfat enthält, zusammen mit den Calcium- und Magnesiumionen des Ansatzwassers ein Niederschlag.
- Der Erfindung liegt die Aufgabe zugrunde, ein Fixierbad zu entwickeln, das frei von Ammoniumionen und EDTA ist, aber die notwendige Fixiergeschwindigkeit aufweist und keine Ablagerungen verursacht.
- Es wurde nun gefunden, daß Komplexbildner der allgemeinen Formel I in ammoniumfreien Fixierbädern keine Ablagerungen verursachen, biologisch abbaubar sind und eine ausreichende Fixiergeschwindigkeit aufweisen.
worin - R
- Wasserstoff, C₁-C₁₀-Alkyl, Hydroxy-C₁-C₁₀-alkyl, C₁-C₁₀-Alkoxy-C₁-C₁₀-alkyl, Carboxy-C₂-C₁₀-alkyl, Dicarboxy-C₁-C₁₀-alkyl, Carboxy-hydroxy-C₁-C₁₀-alkyl, Hydroxy-C₁-C₅-alkyl-(oxy-C₁-C₅-alkyl)n, C₁-C₅-Alkoxy-C₁-C₅-alkyl-(oxy-C₁-C₅-alkyl)n,
- M
- Wasserstoff, Lithium, Natrium, Kalium und
- n
- 1, 2, 3 oder 4 bedeuten.
- Vorzugsweise werden in dem erfindungsgemäßen Fixierbad Komplexbildner der Formel I eingesetzt, in denen
- R
- 1-Carboxy-ethyl oder 1-Hydroxy-ethyl und
- M
- Natrium bedeuten.
- Üblicherweise werden die Komplexbildner in einer Konzentration von 0,5 bis 100 mmol/l verwendet, wobei die Erfindung in einer bevorzugten Form 2 bis 30 mmol/l an Komplexbildner enthält.
- Der unerwartete und überraschende Effekt der Erfindung liegt darin, daß in ammoniumfreien Fixierbädern die erfindungsgemäße Gruppe von abbaubaren Komplexbildnern mit den Calcium- und Magnesiumionen des Ansatzwassers keinen Niederschlag bildet. Andere abbaubare Komplexbildner, wie z.B. NTA, ergeben schon nach wenigen Tagen Stehzeit feste Ausfällungen.
- Das erfindungsgemäße Fixierbad eignet sich insbesondere für farbfotografische Silberhalogenidaufzeichnungsmaterialien, die auf einem reflektierenden oder transparenten Träger (z.B. beidseitig mit Polyethylen beschichtetes Papier oder Cellulosetriacetatfilm) wenigstens eine blauempfindliche, wenigstens eine grünempfindliche und wenigstens eine rotempfindliche Silberhalogenidemulsionsschicht, denen in der angegebenen Reihenfolge wenigstens ein Gelbkuppler, wenigstens ein Purpurkuppler und wenigstens ein Blaugrünkuppler zugeordnet sind, enthalten.
- Das erfindungsgemäße Fixierbad wird innerhalb des üblichen Verarbeitungsverfahrens für fotografische Silberhalogenidmaterialien eingesetzt.
- Das Verarbeitungsverfahren läßt sich unter ständigem Regenerieren der einzelnen Verarbeitungsbäder kontinuierlich ausführen.
- Die in den Beispielen aufgeführten Fixierbäder sind in ihrem Fixierverhalten einem herkömmlichen EDTA-haltigen Fixierbad vergleichbar.
- Ein Fixierbad nachfolgender Zusammensetzung mit genau definierter Calciumionenkonzentration wurde hergestellt und mit verschiedenen Komplexbildnern in unterschiedlichen Konzentrationen versetzt (Tabelle 1). Alle erfindungsgemäßen Fixierbäder zeigten während des Beobachtungszeitraums von 120 Tagen keinen Niederschlag. Die Fixierbäder wurden in offenen Gefäßen bei Raumtemperatur gelagert. Eine Volumenabnahme durch Verdunsten wurde durch periodisches Auffüllen der Bäder mit entionisiertem Wasser ausgeglichen.
Fixierbad: Wasser(entionisiert) 800 ml Natriumsulfat 10g Natriumsulfit 20 g Natriumthiosulfat 60 g Calciumchloridlösung (80 g/l) 5 ml Komplexbildner Siehe Tabelle 1
pH-Wert auf 8 einstellen und mit entionisiertem Wasser auf 1 Liter auffüllen.
Claims (3)
- Ammoniumfreie Fixierbäder, in denen die für die Fixage erforderlichen Wirk- und Hilfsstoffe enthalten sind, dadurch gekennzeichnet, daß sie zusätzlich einen Komplexbildner der Formel I,
R Wasserstoff, C₁-C₁₀-Alkyl, Hydroxy-C₁-C₁₀-alkyl, C₁-C₁₀-Alkoxy-C₁-C₁₀-alkyl, Carboxy-C₂-C₁₀-alkyl, Dicarboxy-C₁-C₁₀-alkyl, Carboxy-hydroxy-C₁-C₁₀-alkyl, Hydroxy-C₁-C₅-alkyl-(oxy-C₁-C₅-alkyl)n, C₁-C₅-Alkoxy-C₁-C₅-alkyl-(oxy-C₁-C₅-alkyl)n,M Wasserstoff, Lithium, Natrium, Kalium undn 1, 2, 3 oder 4 bedeuten, enthalten. - Ammoniumfreie Fixierbäder nach Anspruch 1, dadurch gekennzeichnet, daß als zusätzlicher Komplexbildner Verbindungen der Formel I eingesetzt werden, in denen R 1-Carboxy-ethyl oder 1-Hydroxy-ethyl oder M Natrium bedeuten.
- Ammoniumfreie Fixierbäder nach Anspruch 1, dadurch gekennzeichnet, daß sie den zusätzlichen Komplexbildner in einer Konzentration von 0,5 bis 100 mmol/l enthalten.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE4037298 | 1990-11-23 | ||
| DE4037298A DE4037298A1 (de) | 1990-11-23 | 1990-11-23 | Fixierbad |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| EP0486909A1 true EP0486909A1 (de) | 1992-05-27 |
| EP0486909B1 EP0486909B1 (de) | 1996-02-21 |
Family
ID=6418797
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| EP91119130A Expired - Lifetime EP0486909B1 (de) | 1990-11-23 | 1991-11-11 | Fixierbad |
Country Status (3)
| Country | Link |
|---|---|
| EP (1) | EP0486909B1 (de) |
| JP (1) | JPH04268552A (de) |
| DE (2) | DE4037298A1 (de) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0591934A1 (de) * | 1992-10-05 | 1994-04-13 | Fuji Photo Film Co., Ltd. | Photographische Verarbeitungszusammensetzung und photographisches Verarbeitungsverfahren |
| US5434035A (en) * | 1993-12-29 | 1995-07-18 | Eastman Kodak Company | Fixer additives used in combination with iron complex based bleaches to improve desilvering |
| US5508150A (en) * | 1993-12-29 | 1996-04-16 | Eastman Kodak Company | Fixer additives used in combination with iron complex based bleaches to prevent iron retention |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3994729A (en) * | 1973-04-06 | 1976-11-30 | Fuji Photo Film Co., Ltd. | Method for processing photographic light-sensitive material |
| WO1980000624A1 (en) * | 1978-09-14 | 1980-04-03 | Eastman Kodak Co | Photographic bleach compositions and methods of photographic processing |
-
1990
- 1990-11-23 DE DE4037298A patent/DE4037298A1/de not_active Withdrawn
-
1991
- 1991-11-11 DE DE59107425T patent/DE59107425D1/de not_active Expired - Fee Related
- 1991-11-11 EP EP91119130A patent/EP0486909B1/de not_active Expired - Lifetime
- 1991-11-19 JP JP3329887A patent/JPH04268552A/ja active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3994729A (en) * | 1973-04-06 | 1976-11-30 | Fuji Photo Film Co., Ltd. | Method for processing photographic light-sensitive material |
| WO1980000624A1 (en) * | 1978-09-14 | 1980-04-03 | Eastman Kodak Co | Photographic bleach compositions and methods of photographic processing |
Non-Patent Citations (3)
| Title |
|---|
| GRANT HAIST 'MODERN PHOTOGRAPHIC PROCESSING VOLUME 2' 1979 , JOHN WILEY AND SONS , NEW YORK * |
| PATENT ABSTRACTS OF JAPAN vol. 11, no. 279 (P-614)(2726) 10. September 1987 & JP-A-62 078 551 ( FUJI PHOTO FILM CO. LTD. ) 10. April 1987 * |
| RESEARCH DISCLOSURE. Nr. 167, März 1978, HAVANT GB Seite 40; ANONYMOUS: 'HARDENING FIXERS' * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0591934A1 (de) * | 1992-10-05 | 1994-04-13 | Fuji Photo Film Co., Ltd. | Photographische Verarbeitungszusammensetzung und photographisches Verarbeitungsverfahren |
| US5434035A (en) * | 1993-12-29 | 1995-07-18 | Eastman Kodak Company | Fixer additives used in combination with iron complex based bleaches to improve desilvering |
| US5508150A (en) * | 1993-12-29 | 1996-04-16 | Eastman Kodak Company | Fixer additives used in combination with iron complex based bleaches to prevent iron retention |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH04268552A (ja) | 1992-09-24 |
| DE59107425D1 (de) | 1996-03-28 |
| DE4037298A1 (de) | 1992-05-27 |
| EP0486909B1 (de) | 1996-02-21 |
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