EP0405238B1 - Composition fixateur photographique granulée et sa préparation - Google Patents

Composition fixateur photographique granulée et sa préparation Download PDF

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Publication number
EP0405238B1
EP0405238B1 EP90111254A EP90111254A EP0405238B1 EP 0405238 B1 EP0405238 B1 EP 0405238B1 EP 90111254 A EP90111254 A EP 90111254A EP 90111254 A EP90111254 A EP 90111254A EP 0405238 B1 EP0405238 B1 EP 0405238B1
Authority
EP
European Patent Office
Prior art keywords
fixative
bleach
granulated
granulate
photographic
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.)
Expired - Lifetime
Application number
EP90111254A
Other languages
German (de)
English (en)
Other versions
EP0405238A1 (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 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:
  • 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 is no different from a second sample made 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.

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  • 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)

Claims (7)

1. Composition photographique granulée de fixage ou de blanchiment et fixage, dont les grains contiennent conjointement un thiosulfate et un bisulfite.
2. Composition photographique granulée de blanchiment et de fixage suivant la revendication 1, contenant en outre un produit granulé d'un complexe de fer-(III) ou d'un sel de complexe de fer-(III).
3. Composition photographique granulée de fixage ou de blanchiment et fixage suivant les revendications 1 et 2, dans laquelle les granules présentent des diamètres moyens de particules d'au moins 150 µm.
4. Composition photographique granulée de fixage ou de blanchiment et fixage suivant les revendications 1 et 2, dans laquelle les granules présentent des diamètres moyens de particules de 150 à 3000 µm.
5. Composition photographique granulée de fixage ou de blanchiment et fixage suivant la revendication 1, dont le produit granulé contient 35 à 85 % en poids de thiosulfate et 5 à 15 % en poids de bisulfite.
6. Composition photographique granulée de fixage ou de blanchiment et fixage suivant la revendication 2, dont le produit granulé contient 30 à 50 % en poids de complexe de fer-(III) ou de sel de complexe de fer-(III).
7. Procédé de préparation d'une composition photographique de fixage ou de blanchiment et fixage sous la forme granulée, qui contient un thiosulfate, caractérisé en ce qu'on broie le thiosulfate conjointement avec un bisulfite et le cas échéant d'autres substances solides de manière que le maximum de la courbe de répartition du diamètre de particules se situe en-dessous de 10 µm, on soumet les particules broyées à une agglomération de poudre, on sèche le produit granulé sous vide, on le mélange éventuellement avec les granules de l'agent de blanchiment et on conditionne le mélange sous emballage étanche à la vapeur d'eau.
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
DE19893920920 DE3920920A1 (de) 1989-06-27 1989-06-27 Granuliertes, fotografisches fixiermittel und seine herstellung
DE3920920 1989-06-27
DE19893933226 DE3933226A1 (de) 1989-10-05 1989-10-05 Granuliertes, fotografisches fixiermittel und seine herstellung
DE3933226 1989-10-05

Publications (2)

Publication Number Publication Date
EP0405238A1 EP0405238A1 (fr) 1991-01-02
EP0405238B1 true 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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Publication number Publication date
EP0405238A1 (fr) 1991-01-02
JPH0339735A (ja) 1991-02-20
US5055384A (en) 1991-10-08
DE59000265D1 (de) 1992-09-24

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