EP0405238A1 - Composition fixateur photographique granulée et sa préparation - Google Patents

Composition fixateur photographique granulée et sa préparation Download PDF

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Publication number
EP0405238A1
EP0405238A1 EP90111254A EP90111254A EP0405238A1 EP 0405238 A1 EP0405238 A1 EP 0405238A1 EP 90111254 A EP90111254 A EP 90111254A EP 90111254 A EP90111254 A EP 90111254A EP 0405238 A1 EP0405238 A1 EP 0405238A1
Authority
EP
European Patent Office
Prior art keywords
granules
bleach
fixing
thiosulfate
granulated
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
Application number
EP90111254A
Other languages
German (de)
English (en)
Other versions
EP0405238B1 (fr
Inventor
Peter Dr. Kühnert
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Agfa Gevaert AG
Original Assignee
Agfa Gevaert AG
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Priority claimed from DE19893920920 external-priority patent/DE3920920A1/de
Priority claimed from DE19893933226 external-priority patent/DE3933226A1/de
Application filed by Agfa Gevaert AG filed Critical Agfa Gevaert AG
Publication of EP0405238A1 publication Critical patent/EP0405238A1/fr
Application granted granted Critical
Publication of EP0405238B1 publication Critical patent/EP0405238B1/fr
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

Links

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
    • G03C5/264—Supplying of photographic processing chemicals; Preparation or packaging thereof
    • G03C5/265—Supplying of photographic processing chemicals; Preparation or packaging thereof of powders, granulates, tablets
    • 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 present invention relates to a granular, photographic fixing agent and a method for producing such a fixing agent which can be quickly dissolved.
  • Photographic fixing agents and bleach-fixing agents usually contain a thiosulfate as the fixing substance, which is intended to dissolve undeveloped silver halide and silver halide which has newly formed by bleaching the metallic silver from the photographic material.
  • thiosulfate ammonium thiosulfate [(NH4) 2S2O3] is largely used due to its fast fixing reaction, but this has a serious disadvantage. Powders of this substance bake when standing, even in the absence of atmospheric moisture, to form solid lumps that have to be crushed with difficulty and are difficult to dose then when the ammonium thiosulfate powder is mixed with the other components of the fixing or bleach-fixing bath.
  • the sodium thiosulfate used as an alternative is also disadvantageous because it dissolves poorly in water and forms crusts on the bottom of the fixing or bleach-fixing bath.
  • the fixing or bleach-fixing agent is largely offered and used in a liquid formulation.
  • this has the disadvantage of increased costs due to the water ballast.
  • the object of the invention is to provide a form of assembly for ammonium thiosulfate which is firm and yet easy to dose and which dissolves quickly in the bath.
  • granulated fixing agents can be prepared by grinding a thiosulfate together with a disulfite and optionally other solid substances such that the maximum of the particle diameter distribution curve is less than 10 ⁇ m, the ground particles are subjected to powder agglomeration and the granules are dried in vacuo , if necessary mixed with the granules of the bleaching agent and packed in a water vapor-tight manner.
  • the granules of the solid components of a photographic fixing or bleach-fixing agent produced in this way are mechanically stable, of uniform grain size, show a high dissolution rate and unlimited durability, are dust-free and free-flowing.
  • Preferred thiosulfates are alkali, in particular sodium, and ammonium thiosulfate.
  • Alkali and ammonium disulfite are suitable as disulfites.
  • the solid constituents are usually comminuted to particle sizes of ⁇ 10 ⁇ m by jet milling.
  • the powder agglomeration is preferably carried out in a fluidized bed, granulation liquid, for example 200 ml of water per kg of powder and, if appropriate, some binder, for example corn starch, being added to the particles to be agglomerated.
  • the average particle diameter of the granules should preferably be ⁇ 150 ⁇ m and is in particular 150 to 3000 ⁇ m.
  • thiosulfate granules are complexing agents such as ethylenediaminetetraacetic acid (EDTA) and agents for adjusting the desired pH such as sodium carbonate.
  • EDTA ethylenediaminetetraacetic acid
  • granules are preferably produced separately from the fixing agent and bleaching agent and mixed with one another.
  • the granules of the bleaching agent contain an iron (III) complex or an iron (III) complex salt, for example an ammonium iron complex salt from EDTA, the propylenediamine tetraacetic acid (PDTA), diethylenetriaminepentaacetic acid (DTPA) or nitrilotriacetic acid (NTA) and optionally free complexing agents, for example EDTA, PDTA, DTPA or NTA.
  • an iron (III) complex or an iron (III) complex salt for example an ammonium iron complex salt from EDTA, the propylenediamine tetraacetic acid (PDTA), diethylenetriaminepentaacetic acid (DTPA) or nitrilotriacetic acid (NTA) and optionally free complexing agents, for example EDTA, PDTA, DTPA or NTA.
  • the granules of the bleaching agent are preferably produced in the same way as the granules of the fixing agent and in particular have an average particle diameter in the same range.
  • the agent according to the invention preferably contains 35 to 85% by weight of thiosulfate, 5 to 15% by weight of disulfite and, in the case of a bleach-fixing agent, 30 to 50% by weight of iron (III) complex or iron (III) complex salt.
  • the bleach-fix bath granules are produced by mixing two individual granules A and B. The following quantities of substance are used per liter of ready-to-use solution: 1.
  • Granules A 1.1 ammonium thiosulfate 75.0 g 1.2 ammonium carbonate 2.6 g 1.3 sodium disulfite 13.5 g 91.1 g 2.
  • Granules B 2.1 Ammonium Iron EDTA 57.0 g 2.2 EDTA acid 0.8 g 57.8 g
  • the chemicals listed under A are - in the specified mixing ratio - crushed in a so-called Alexander mill to about 1 mm grain size and then in an air jet mill to a particle size of 5 ⁇ m, ground.
  • the ground material is then granulated in portions of approximately 500 grams on a commercially available fluidized bed granulator (Strea-1 laboratory device from Aeromatic, Bubendorf / Switzerland).
  • the colorless product obtained does not clump and is non-dusting and free-flowing.
  • the chemicals listed under B are mixed and granulated in the same granulator (as in A) by spraying on 50% by weight ammonium iron EDTA solution, which contains excess ammonia, in about 7 minutes. 200 ml of this solution are sprayed onto 600 g of mixture B at room temperature.
  • Granules A and B are mixed to produce the ready-to-use mixed granulate.
  • the mixture of 91.1 g of granules A and 57.8 g of granules B gives the amount of mixed granules required for 1 liter of bleach-fixing bath.
  • the mixed granulate is free-flowing, free-flowing and non-dusting. With stirring, it dissolves in water at room temperature in 45 seconds to a dark red solution. This does not differ from a second sample, which was prepared from the same amount of the corresponding powdered chemicals.
  • the mixed granulate, packed airtight and moisture-proof, has an unlimited shelf life.
  • the photographic effectiveness corresponds entirely to a bleach-fix bath which was produced from non-granulated chemicals according to the same recipe.
  • the mixture After comminution in the so-called Alexander mill, the mixture is ground in an air jet mill to an average particle size of approximately 5 ⁇ m.
  • the colorless granules are dust-free, free-flowing and non-clumping. Sealed in aluminum-coated bags, it has an unlimited shelf life. It dissolves in water with stirring within about 10 seconds to a colorless and clear solution with a pH of 7.3.
  • this solution corresponds entirely to a second one, which was produced from the same chemicals without granulation using the same recipe.

Landscapes

  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Detergent Compositions (AREA)
  • Silver Salt Photography Or Processing Solution Therefor (AREA)
EP90111254A 1989-06-27 1990-06-14 Composition fixateur photographique granulée et sa préparation Expired - Lifetime EP0405238B1 (fr)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
DE3933226 1989-05-10
DE3920920 1989-06-27
DE19893920920 DE3920920A1 (de) 1989-06-27 1989-06-27 Granuliertes, fotografisches fixiermittel und seine herstellung
DE19893933226 DE3933226A1 (de) 1989-10-05 1989-10-05 Granuliertes, fotografisches fixiermittel und seine herstellung

Publications (2)

Publication Number Publication Date
EP0405238A1 true EP0405238A1 (fr) 1991-01-02
EP0405238B1 EP0405238B1 (fr) 1992-08-19

Family

ID=25882361

Family Applications (1)

Application Number Title Priority Date Filing Date
EP90111254A Expired - Lifetime EP0405238B1 (fr) 1989-06-27 1990-06-14 Composition fixateur photographique granulée et sa préparation

Country Status (4)

Country Link
US (1) US5055384A (fr)
EP (1) EP0405238B1 (fr)
JP (1) JPH0339735A (fr)
DE (1) DE59000265D1 (fr)

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EP0538793A1 (fr) * 1991-10-21 1993-04-28 Fuji Photo Film Co., Ltd. Kit pour le traitement photographique
EP0569852A1 (fr) * 1992-05-13 1993-11-18 Fuji Photo Film Co., Ltd. Composition de blanchiment-fixage pour produit photographique couleur et procédé de traitement de produit photographique couleur avec cette composition
EP0580372A2 (fr) * 1992-07-16 1994-01-26 Konica Corporation Composé pour traitement photographique, noir et blanc
EP0624821A1 (fr) * 1993-05-10 1994-11-17 Konica Corporation Comprimé pour le traitement d'un matériau photographique couleur à l'halogénure d'argent sensible à la lumière
US5366853A (en) * 1991-11-06 1994-11-22 Konica Corporation Tablet-shaped processing agent and method for processing silver halide photographic light sensitive materials
US5780211A (en) * 1991-05-01 1998-07-14 Konica Corporation Processing composition in the tablet form for silver halide photographic light-sensitive material

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DE69127249T2 (de) * 1990-10-02 1997-12-04 Fuji Photo Film Co Ltd Verfahren zur Verarbeitung eines farbphotographischen Silberhalogenidmaterials
EP0518541B1 (fr) * 1991-05-31 2000-09-13 Konica Corporation Méthode de traitement de matériau photographique blanc et noir à l'halogénure d'argent sensible à la lumière
JPH0593989A (ja) * 1991-10-03 1993-04-16 Konica Corp 写真用処理剤の包装材料
US5270154A (en) * 1992-01-31 1993-12-14 Fuji Hunt Photographic Chemicals Inc. Method of making flowable alkaline thiosulfate/alkaline sulfite and the product thereof
JPH05289248A (ja) * 1992-04-08 1993-11-05 Konica Corp 写真用処理剤
JPH0643604A (ja) * 1992-07-25 1994-02-18 Konica Corp ハロゲン化銀写真感光材料の処理方法
JPH0659404A (ja) * 1992-08-12 1994-03-04 Konica Corp ハロゲン化銀写真感光材料の現像処理方法及び処理剤
JP2934997B2 (ja) * 1993-01-21 1999-08-16 コニカ株式会社 黒白ハロゲン化銀写真感光材料の処理方法
US5480768A (en) * 1993-02-17 1996-01-02 Konica Corporation Method for processing exposed silver halide photographic light-sensitive material using a solid processing composition replenisher
US5409805A (en) * 1993-07-29 1995-04-25 Konica Corporation Solid processing agent for silver halide photographic light-sensitive materials
US5557362A (en) 1994-06-16 1996-09-17 Konica Corporation Silver halide photosensitive material automatic developing apparatus
JPH0869098A (ja) 1994-08-31 1996-03-12 Konica Corp ハロゲン化銀写真感光材料用自動現像機
US5624793A (en) * 1994-11-11 1997-04-29 Konica Corporation Method of manufacturing solid processing composition for silver halide photographic light-sensitive materials
JPH08160588A (ja) 1994-12-06 1996-06-21 Konica Corp ハロゲン化銀写真感光材料用自動現像機
US5618658A (en) * 1995-02-22 1997-04-08 Fuji Hunt Photographic Chemicals, Inc. Process for producing an ammonium thiosulfate product
JP3574986B2 (ja) 1996-01-16 2004-10-06 コニカミノルタホールディングス株式会社 ハロゲン化銀写真感光材料用固体処理剤及びハロゲン化銀写真感光材料の処理方法
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Citations (2)

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GB1099790A (en) * 1966-02-01 1968-01-17 Goldschmidt Ag Th Flowable ammonium thiosulfate and method for its manufacture
DE1911609A1 (de) * 1969-03-07 1970-09-17 Hoechst Ag Stabilisiertes Ammoniumthiosulfat

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JPS54133332A (en) * 1978-04-07 1979-10-17 Oriental Photo Ind Co Ltd Preparation of powdered bleaching agent for photograph
JPS6132848A (ja) * 1984-07-26 1986-02-15 Konishiroku Photo Ind Co Ltd 写真処理剤封入袋
JP2556339B2 (ja) * 1987-09-29 1996-11-20 コニカ株式会社 長期処理安定性を有する写真処理剤及び写真感光材料の処理方法
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Publication number Priority date Publication date Assignee Title
GB1099790A (en) * 1966-02-01 1968-01-17 Goldschmidt Ag Th Flowable ammonium thiosulfate and method for its manufacture
DE1911609A1 (de) * 1969-03-07 1970-09-17 Hoechst Ag Stabilisiertes Ammoniumthiosulfat

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5780211A (en) * 1991-05-01 1998-07-14 Konica Corporation Processing composition in the tablet form for silver halide photographic light-sensitive material
EP0538793A1 (fr) * 1991-10-21 1993-04-28 Fuji Photo Film Co., Ltd. Kit pour le traitement photographique
US5366853A (en) * 1991-11-06 1994-11-22 Konica Corporation Tablet-shaped processing agent and method for processing silver halide photographic light sensitive materials
EP0569852A1 (fr) * 1992-05-13 1993-11-18 Fuji Photo Film Co., Ltd. Composition de blanchiment-fixage pour produit photographique couleur et procédé de traitement de produit photographique couleur avec cette composition
EP0580372A2 (fr) * 1992-07-16 1994-01-26 Konica Corporation Composé pour traitement photographique, noir et blanc
EP0580372A3 (en) * 1992-07-16 1995-08-23 Konishiroku Photo Ind Black-and-white photographic processing compound
EP0624821A1 (fr) * 1993-05-10 1994-11-17 Konica Corporation Comprimé pour le traitement d'un matériau photographique couleur à l'halogénure d'argent sensible à la lumière

Also Published As

Publication number Publication date
JPH0339735A (ja) 1991-02-20
EP0405238B1 (fr) 1992-08-19
US5055384A (en) 1991-10-08
DE59000265D1 (de) 1992-09-24

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