EP0224858B1 - Method for processing silver halide color photographic light-sensitive material - Google Patents

Method for processing silver halide color photographic light-sensitive material Download PDF

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Publication number
EP0224858B1
EP0224858B1 EP19860116372 EP86116372A EP0224858B1 EP 0224858 B1 EP0224858 B1 EP 0224858B1 EP 19860116372 EP19860116372 EP 19860116372 EP 86116372 A EP86116372 A EP 86116372A EP 0224858 B1 EP0224858 B1 EP 0224858B1
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EP
European Patent Office
Prior art keywords
solution
tank
stabilizing
dialyzing
processing
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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.)
Expired - Lifetime
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EP19860116372
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German (de)
English (en)
French (fr)
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EP0224858A2 (en
EP0224858A3 (en
Inventor
Naoki Takabayashi
Syozo Aoki
Shigeharu Koboshi
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Konica Minolta Inc
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Konica Minolta Inc
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Publication of EP0224858A2 publication Critical patent/EP0224858A2/en
Publication of EP0224858A3 publication Critical patent/EP0224858A3/en
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Publication of EP0224858B1 publication Critical patent/EP0224858B1/en
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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
    • G03C7/3046—Processing baths not provided for elsewhere, e.g. final or intermediate washings
    • 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
    • G03C5/395—Regeneration of photographic processing agents other than developers; Replenishers therefor
    • G03C5/3956—Microseparation techniques using membranes, e.g. reverse osmosis, ion exchange, resins, active charcoal

Definitions

  • the present invention relates to a method for processing a silver halide light-sensitive material (hereinafter referred to as "the light-sensitive material”) and more particularly to a method for processing the light-sensitive material in a stabilized state, subsequent to a desilverization process.
  • the light-sensitive material a silver halide light-sensitive material
  • the replenishing amount of a stabilizing solution is in the order of about 2.5l ⁇ 25 ml per 1 m2 of the light-sensitive material and more preferably in the order of 200 ml ⁇ 50 ml.
  • a first object of the present invention is to provide a color stabilization method which does not involve any problem by reducing the concentration of fixing and bleach-fixing components in a stabilizing solution.
  • a second object of the present invention is to provide a color stabilization method which does not increase the generation of yellow stains immediately after processing an unexposed portion of a light-sensitive material even when the material is continuously processed for a prolonged period of time.
  • a third object of the present invention is to provide a method for reducing the replenishing amount of the stabilizing solution or for re-using the solution by removing harmful components contained in the solution.
  • a method for processing a silver halide photographic light-sensitive material comprising the steps of treating the silver halide photographic light-sensitive material with a solution capable of fixing the material and then treating it with a stabilizing solution with a part of the stabilizing solution being dialytically treated without electrical current by a dialysis means including a charge-mosaic membrane.
  • the stabilizing solution contains a chelating agent whose stability constant with respect to ferric ion is not less than 6.
  • Fig. 1 is a conceptual view of a dialyzing tank using a charge mosaic membrane and attached to a photographic processing apparatus and Figs. 2 and 3 are conceptual views of one embodiment of a dialyzing tank using a charge-mosaic membrane.
  • the fixing and bleach-fixing components in the stabilizing solution an eluent from the light-sensitive material and fatigued components in the stabilizing solution are all washed out by the rinsing step but if the material is subjected to a direct stabilization process without the rinsing step, all of the components will accumulate in the stabilizing solution so that yellow stains generate on the light-sensitive material immediately after the processing thereof or due to the storage thereof.
  • the dialysis through a dialyzing means using a charge mosaic membrane is a processing method comprising the steps of introducing a stabilizing solution into a demineralization chamber which is separated from a dialysis chamber through a charge mosaic-membrane within a processing tank and introducing a dialyzing solution into the dialysis chamber.
  • the charge-mosaic membrane referred to in the present invention is such type of membrane in which anion exchange zones and cation exchange zones are alternately separated by neutral zones and preferably, the anion exchange zones and cation exchange zones on one of the surface of the membrane extend through the other surface.
  • the charge mosaic membrane and the demineralization chamber constitute one cell, to provide a plurality of such cells is effective in view of reducing the area of installation of the processing apparatus and the number of cells may be determined by the amount of the stabilizing solution to be processed and the area of installation of the processing apparatus.
  • the dialyzing solution may be water or water added with salt in a desired amount. Further, it is preferable to recover silver from the dialyzing solution but the stabilizing solution after the recovery of silver may be used for the process according to the present invention.
  • a method of collecting silver from the dialyzing solution an electrodialysis method, electrolysis method or ion exchange method may be used. Further, it is preferable to perform demineralization by the dialyzing solution and in this case, the dialysis method, a method for bringing silver into contact with ion exchange resin, activated carbon or zeolite or a method for precipitating by adding to the dialyzing solution such type of salt that is liable to become insoluble may be used solely or in combinations of more than two of them.
  • the stabilizing solution to be introduced into the demineralization chamber may be pretreated by ion exchange resin, chelating exchange resin, activated carbon and zeolite solely or in combinations of more than two of them thereby improving the durability of the charge-mosaic membrane.
  • the charge-mosaic membrane used in the present invention may include anion exchange zones and cation exchange zones in a polka-dotted fashion or may include anion exchange zones, neutral zones and cation exchange zones in the form of stripes when the horizontal surface of the membrane is viewed from above.
  • the charge mosaic membrane given in J. Memb. Sci., Vol. 20, P313, 1984 may be used.
  • the stabilizing solution of the present invention contains a chelating agent whose chelating stability constant with respect to ferric ion is not less than 6.
  • chelating stability constant referred to herein is used in the meaning generally known from L.G. Sillen and A. E. Martell's "Stability Constants of Metal-ion Complexes” published by the Chemical Society, London (1964) and S. Chaberek and A. E. Martell's "Organic Sequestering Agents” published by Wiley (1959).
  • chelating agents whose chelating stability constant with respect to ferric ion is not less than 6, there are an organic carbonic acid chelating agent, organic phosphoric acid chelating agent, condensed phosphoric acid chelating agent and polyhydroxylic compound.
  • chelating agents whose chelating stability constant with respect to ferric ion is not less than 13 among which there are ethylenediamine diorthohydroxyphenyl acetate, nitrilotriacetic acid, hydroxyethylenediamine triacetate, diethylenetriamine pentaacetate, hydroxyethylimino diacetate, diaminopropanol tetraacetate, transcyclohexenediamine tetraacetate, ethylenediamine tetrakismethylene phosphonic acid, nitrilotrimethylene phosphonic acid, 1- hydroxyethylidene-1, 1-diphosphonic acid, 1, 1- diphosphonoethane- 2-carboxylic acid, 2- phosphonobutane-1, 2, 4-tricarboxylic acid, 1- hydroxy- 1- phosphonopropane- 1, 2, 3-tricarboxylic acid, catechol- 3, 5- disulphonic acid, sodium pyrophosphate,
  • a pH adjuster sodium benzoate, butyl hydroxybenzoic acid, antibiotic substances, an anti-molding agent, a preservative, a dispersant, a hardening agent and an optical brightening agent.
  • the most effective additive is the ammonium compounds described in the specification of the Japanese Patent Application No. 58693/1983.
  • the processing temperature for the stabilization process is in the order of 15°C ⁇ 60°C, preferably 20°C ⁇ 45°C. Further, it is preferable that the processing time be as short as possible in view of speedy processing and it is usually in the order of 20 sec ⁇ 10 min with the range of 45 sec ⁇ 5 min being the most preferable.
  • the processing time by the first-stage tank may be made the same as that by the last-stage tank or the time by the latter tank may be made shorter than that by the former tank but in this case, it is preferable that the processing time by the last-stage tank be made longer.
  • the processing time by the last-stage tank is preferably made longer by 20 ⁇ 50% than that by the first-stage tank and further, it is preferable that the stabilization processing be performed by multi-stage tanks and a reverse flow system in which the replenisher is supplied from the last-stage tank so as to make it overflow the first-stage tank in sequence be employed.
  • the rinsing and surface washing of the light-sensitive material with a small amount of water for a short time can be performed at choice as occasion demands.
  • the processing solutions having a fixing capability are those which are adopted for desilverization and among them are included a fixing solution and a bleach fixing solution.
  • the generally used fixing agent is thiosulfate.
  • a light-sensitive material is processed by the processing solution having a fixing capabilities and subsequently processed with the stabilizing solution
  • a silver recovering bath and a rinsing means may be provided between the processing by the fixing solution (bath) or bleach-fixing solution (bath) and the processing by the stabilizing solution.
  • the method for bringing the stabilizing solution into contact with a light-sensitive material according to the present invention is favorably performed by dipping the light-sensitive material in the solution as in the case of the general processing solutions but the stabilizing solution may be applied to the emulsion coated surface of the light-sensitive material, both surfaces of the carriage leader and the transfer belt by means of a sponge or synthetic resin cloth, or sprayed by means of a sprayer.
  • the stabilizing solution which has been used for treating the light-sensitive material.
  • One of the methods is such that a tank having a charge mosaic membrane and a dialyzing solution is provided in a stabilizing bath so as to continuously treat the stabilizing solution and the other is that an overflowed waste solution from the stabilizing bath is treated by a dialyzing tank using a charge-mosaic membrane and then returned to the stabilizing bath but the second method is more preferable than the first method.
  • the stabilizing solution is treated by the tank including the charge-mosaic membrane and the dialyzing solution, it is preferable that the dialyzing solution be circulated constantly. Further, in case the overflowed solution from the stabilizing bath is introduced into the dialyzing tank, the stabilizing solution to be introduced into the demineralization chamber in the dialyzing tank and the dialyzing solution to be introduced into the dialyzing chamber are constantly circulated.
  • the stabilizing process of the present invention is performed in one or more than two stabilization tanks.
  • a dialyzing device using a charge-mosaic membrane may be provided in each of the tanks but in that case, it is desirable to connect it to the stabilizing tank adjacent a processing bath having a fixing capacity.
  • an overflow from the bath is processed by the dialyzing device using the charge mosaic membrane, it is possible to process the overflow from the stabilizing tank adjacent the processing tank having a fixing capacity and such overflow may be reused as another stabilizing solution after processing.
  • the light-sensitive material should be color-developed and a color image should be formed by coupling reactions between the oxide of the principal color developing ingredient and the color coupler and that in case "the processing solution having a fixing capacity" according to the present invention contains a fixing component without a bleaching component, the material should be subjected to bleaching after the color developing process.
  • the generally known techniques can be used without any specific limitations and it is also possible to refer to the techniques described in the Japanese Patent O.P.I. Publication Nos. 14834/1983, 105145/1983, 134634/1983 and 18631/1983, and Japanese Patent Application No 2709/1983 all of which were filed by the subject applicant.
  • it is particularly preferable to make the stabilizing solution of the present invention contain as anti-molding agent and the descriptions in the above publications can also be referred to for obtaining techniques on, and other compositions or examples of, the anti-molding agent.
  • Fig. 1 is a conceptual view showing one example of a stabilizing solution processing step using a dialyzing means having a charge mosaic membrane according to the present invention.
  • reference numeral 11 designates a light-sensitive material processing apparatus which comprises a color developing tank 1, a bleach-fixing solution tank 2, a first stabilizing solution tank 3, a second stabilizing solutions tank 4 and a third stabilizing solution tank 5.
  • An image-exposed light-sensitive material is transferred along a passage shown by the chain-line, stabilized through the first, second and third stabilizing solution tank after it is developed and bleach-fixed and then dried at a drying section (not shown).
  • Reference numeral 6 designates a dialyzing tank the interior of which is divided into a demineralization chamber 7 and a dialysis chamber 9 by means of a charge-mosaic membrane 8.
  • a stabilizing solutions in the first stabilizing solution tank 3 and in the dialysis chamber 9 into which the dialyzing solution D is flowed. Further, the unnecessary components in the stabilyzing solution moves in the dialyzing solution through the charge-mosaic membrane so that the stabilizing solution is kept effective.
  • Fig. 2 is a diagrammatical view of a dialyzing tank in which a plurality of demineralization chambers 7 and a plurality of dialyzing chambers 9 are separated by a plurality of charge-mosaic membranes with the chambers 7 and 9 being arranged in an alternative fashion and
  • Fig. 3 is an example of a dialyzing tank provided with spacers 10 in the vicinity of a charge-mosaic membrane 8 which spacers are adopted to generate a turbulent flow in a stabilyzing solutions or a dialyzing solution D. In any of the above two cases, it is possible to obtain a high dialyzing efficiency.
  • SAKURA color papers prepared by Konishiroku Photo Ind. Co., Ltd.
  • a color developing tank solution Benzil alcohol 15 ml Ethylene glycol 15 ml Potassium sulfite 2.0 g Potassium bromide 1.3 g Sodium chloride 0.2 g Potassium carbonate 30.0 g Hydroxylamine sulfate 3.0 g Polyphosphoric acid (TPPS) 2.5 g 3- methyl- 4- amino- N-ethyl- N- ( ⁇ -methanesulfonamide ethyl)-aniline sulfite 5.5 g optical brightening agent (4, 4'-diaminostilbene disulfonic acid derivative) 1.0 g Catechol-3, 5-disulfonic acid 0.3 g water to make 1 l and adjusted to pH 10.50 with KOH.
  • a bleach-fixing tank solution Ferric ammonium ethylenediamine tetraacetate dihydrate 60 g Ethylenediamine tetraacetate 3 g Ammonium thiosulfate (70% solution) 100 ml Ammonium sulfite (40% solution) 27.5 ml water to make 1 l and adjusted to pH 7.1 with potassium carbonate or glacial acetic acid.
  • a bleach-fixing replenisher A Ferric ammonium ethylenediamine tetraacetate dihydrate 260 g Potassium carbonate 42 g Water to make 1 l and adjusted to pH 6.7 ⁇ 0.1.
  • a bleach-fixing replenisher B Ammonium thiosulfate (70% solution) 500 ml Ammonium sulfite (40% solution) 150 ml Ethylenediamine tetraacetic acid 17 g Glacial acetic acid 85 ml Water to make 1 l and adjusted to pH 4.6 ⁇ 0.1.
  • the above mentioned color development tank solution, bleach-fixing tank solution and stabilizing tank solution were filled into an automatic developing machine and an image-wise exposed color paper is continuously processed by replenishing the above-mentioned color developing replenisher solution, the bleach-fixing solutions A and B and the stabilizing solution every three minutes by using quantitative cups.
  • the replenishing amounts of the solutions were that the amount of the color developing replenisher solution into the color developing tank was 170 ml, those of the bleach-fixing solutions A and B into the bleach-fixing tank were each 25 ml and the amounts of the replenisher into the stabilization processing tank in three cases were 100 ml, 300 ml and 1 l, respectively.
  • the automatic developing machine was made to include a first tank, a second tank and a third tank arranged in that order in the direction of the flow of the light-sensitive material and a multistage counter-flow system was adopted in which an overflow from the last tank was flowed into the second tank and an overflow from the second tank was flowed into the first tank.
  • the above continuous processing was performed until the entire replenishing amount of the stabilizing solution became three times the volume of the stabilizing solution tank and the unexposed color paper was processed to make a sample. Further, a comparison or reference sample processed by replacing the stabilization process with rinsing by running water was prepared.
  • the reflectance of the samples were measured by a wavelength of 445 nm for examining the generation of yellow stains on the day of processing with the results shown in Table 1. Further, to test the generation of yellow stains after ageing, the samples were stored for 25 days at a temperature of 70°C and 80% RH and then the resultant yellow stains were measured with blue light by using an optical densitomer (PDA -65 of Konishiroku Photo Ind. Co.,Ltd.) with the results shown in Table 1.
  • PDA -65 of Konishiroku Photo Ind. Co.,Ltd.
  • the present invention is extremely effective because no problem occurs even when the replenishing amount of the stabilizing solution is reduced.
  • a stabilizing tank solution and a stabilizing replenisher 1- hydroxyethylidine- 1, 1- diphosphonic acid 0.5 g Bismuth chloride (45% aqueous solution) 0.1 g Magnecium sulfate 0.04 g Ammoniam water (25% aqueous solution) 2.0 g 5- chloro- 2 methyl- 4- isothiazoline 3- on 0.02 g 2- methyl- 4- isothiazoline- 3- on 0.02 g 2- octyl- 4- isothiazoline- 3- on 0.01 g Orthophenylphenol sodium salt 0.03 g Water to make 1 l and adjusted to pH 7.0 with sulfuric acid.
  • the above stabilizing solution was used in place of the stabilizing solution and replenisher in the example-1 and a color paper was continuously processed in the same manner as the experiment-1 of the example-1 with a replenishing amount of 750 ml per 1 m2 of the color paper.
  • a recycling system was adopted in which an overflow from the stabilizing both was used to solve the replenisher and the rate of generation of yellow stains was obtained by the same experiments as those of the example-1 with the results shown in the Table 2.
  • the dialyzing tank using the charge mosaic membrane shown in Fig. 1 was directly connected to the first tank as in the case of the experiment-2 of the example-1 and an unexposed color paper was continuously processed until the entire amount of the replenisher became three times the volume of the stabilizing bath tanks. Then an experiment same as the experiment-1 of the example-1 was conducted to obtain samples and the rates of generation of yellow stains on the samples on the day of processing and after storage thereof were obtained with the results shown in the Table 3.
  • the replenishing amount of the stabilizing solution was 100 ml per 1 m2 of the light-sensitive material and to obtain a reference example, the same experiment was conducted by using the No. 3 stabilizing solution prescribed in the Table 3 and without performing a dialyzing process with the charge-mosaic membrane, with the results shown in the Table 3.
  • the effects of the present invention are outstanding when the stabilizing solutions which are added with the chelating agents Nos. 7 through 12, especially Nos. 7, 8 and 9 are used and the solution added with the chelating agent No. 7 (1- hydroxyethylidene- 1, 1-diphosphonic acid) is the most preferable.
  • the chelating agents Nos. 11 and 12 containing ammonia water are preferable with the latter (No. 12) containing both ammonia water and 1- hydroxyethylidene- 1, 1-phosphonic acid being particularly preferable.
  • the processing time with the stabilizing bath tank was not changed.
  • the stabilizing solution in the first tank was processed by a dialyzing tank having a charge-mosaic membrane, the same results as those of the examples 2 and 3 were obtained.
  • the dialyzing tank with charge mosaic membrane was not used for the single stabilizing tank, it was found that the rate of generation of yellow stains became quite outstanding and this tendency was also observed after the sample was stored.
  • the dialyzing tank in Fig.2 was used. As a result, it was found that even when the dialyzing time was six hours, the rate of generation of yellow stains was substantially the same as a case when the dialyzing time was twenty hours with the use of the dialyzing tank in Fig. 1. This phenomenon is likely due to the fact that the dialyzing speed was increased as compared to that in the case of the dialyzing tank in Fig. 1.
  • the following first stabilizing solution for a negative was processed by use of the dialyzing tank of the present invention and it was found that no yellow stain generated on the negative and the replenishing amount of the stabilizing solution could be reduced to a considerable degree.

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  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Engineering & Computer Science (AREA)
  • Water Supply & Treatment (AREA)
  • Silver Salt Photography Or Processing Solution Therefor (AREA)
EP19860116372 1985-11-27 1986-11-25 Method for processing silver halide color photographic light-sensitive material Expired - Lifetime EP0224858B1 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP27032185A JPS62127740A (ja) 1985-11-27 1985-11-27 ハロゲン化銀カラ−写真感光材料の処理方法
JP270321/85 1985-11-27

Publications (3)

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EP0224858A2 EP0224858A2 (en) 1987-06-10
EP0224858A3 EP0224858A3 (en) 1989-04-05
EP0224858B1 true EP0224858B1 (en) 1993-06-30

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EP19860116372 Expired - Lifetime EP0224858B1 (en) 1985-11-27 1986-11-25 Method for processing silver halide color photographic light-sensitive material

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EP (1) EP0224858B1 (ja)
JP (1) JPS62127740A (ja)
AU (1) AU580198B2 (ja)

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5055382A (en) * 1989-02-01 1991-10-08 Long John J Bleach-fix regeneration kit and use thereof in photographic processing
WO1991005289A1 (en) * 1989-09-29 1991-04-18 Eastman Kodak Company Rinse bath for use in photographic processing
JP2676638B2 (ja) * 1989-12-28 1997-11-17 富士写真フイルム株式会社 ハロゲン化銀カラー写真感光材料の処理方法

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS60220345A (ja) * 1984-04-17 1985-11-05 Konishiroku Photo Ind Co Ltd ハロゲン化銀カラ−写真感光材料の処理方法
JPS6128949A (ja) * 1984-05-16 1986-02-08 Konishiroku Photo Ind Co Ltd ハロゲン化銀カラ−写真感光材料の処理方法

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AU580198B2 (en) 1989-01-05
AU6572086A (en) 1987-06-04
EP0224858A2 (en) 1987-06-10
JPS62127740A (ja) 1987-06-10
JPH0562975B2 (ja) 1993-09-09
EP0224858A3 (en) 1989-04-05

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