EP0590364A2 - Verfahren und Vorrichtung zur Verarbeitung eines lichtempfindlichen Aufzeichnungsmaterials für gerbende Entwicklung - Google Patents

Verfahren und Vorrichtung zur Verarbeitung eines lichtempfindlichen Aufzeichnungsmaterials für gerbende Entwicklung Download PDF

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Publication number
EP0590364A2
EP0590364A2 EP93114390A EP93114390A EP0590364A2 EP 0590364 A2 EP0590364 A2 EP 0590364A2 EP 93114390 A EP93114390 A EP 93114390A EP 93114390 A EP93114390 A EP 93114390A EP 0590364 A2 EP0590364 A2 EP 0590364A2
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EP
European Patent Office
Prior art keywords
wash
bath
filter
liquid
out liquid
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.)
Withdrawn
Application number
EP93114390A
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German (de)
English (en)
French (fr)
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EP0590364A3 (enrdf_load_stackoverflow
Inventor
Manfred Franz Klaus Patzelt
Herrmann Knapp
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
DuPont de Nemours Deutschland GmbH
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Application filed by DuPont de Nemours Deutschland GmbH filed Critical DuPont de Nemours Deutschland GmbH
Publication of EP0590364A2 publication Critical patent/EP0590364A2/de
Publication of EP0590364A3 publication Critical patent/EP0590364A3/xx
Withdrawn legal-status Critical Current

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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
    • 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
    • G03C5/3952—Chemical, mechanical or thermal methods, e.g. oxidation, precipitation, centrifugation
    • 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
    • G03C5/29—Development processes or agents therefor
    • G03C5/315—Tanning development

Definitions

  • the invention relates to a method and a device for processing an exposed, tannable developable light-sensitive material which contains at least one of its layers at least uncured gelatin, a light-sensitive silver halide, a pigment and a tanning developer substance.
  • Image recording methods are known in which a photosensitive recording layer containing uncured gelatin as a binder for a silver halide can be imagewise cured by exposure and development with a tanning developer. The uncured non-image parts can then be washed out of the layer with a liquid, for example with warm water, whereby the image is created as a relief.
  • the layer still contains a strongly coloring pigment such as carbon black, an image of sufficient density can be obtained even with a small layer thickness or relief depth. It is also known to incorporate the tanning developer into the recording material so that only an alkaline activator is required for development.
  • washout liquid When washing out, the components of the non-image areas of the recording layer pass almost completely into the washout liquid. These include unexposed silver halide, binder components and possibly the tanning developer. Therefore, the used one Wash-out liquid is no longer simply put into the sewage system as waste water.
  • DE 28 32 530-C2 describes light-sensitive materials for tanning development and processing methods therefor.
  • the exposed material is treated with an alkaline tanning developer or activator and then washed out with warm water.
  • An acetic acid stop bath can be used between development and washing out. None is said about the treatment of the used wash-out water.
  • a device for treating tannin-developable recording materials is sold by the applicant under the name DP 26 WOLF® and is shown in the company publication “WOLF® Wash-Off System” (April 1989). It contains an activator tank to hold an alkaline activator bath, a fixer tank for the fixer bath, a washout tank and a dryer.
  • the wash-out liquid in the sump of the wash-out tank is pressed into the spray nozzles by a high-pressure pump with a delivery rate of approx. 50 l per minute, sprayed onto the developed recording material, washes out its untanned areas and collects again in the sump.
  • a coarse filter in the wash liquid circuit prevents solid particles from clogging the spray nozzles. To avoid that the washed out components of the Unlimited accumulation of recording layers in the wash-out liquid, a considerable part of the liquid is continuously removed as wastewater from the circuit and replaced by warm fresh water.
  • the known processing and washing-out processes for tanned materials are still unsatisfactory.
  • the silver-containing fixer is dragged into the wash-out section and causes the wastewater to still be excessively loaded with dissolved silver.
  • the washout process itself requires relatively large amounts of water, for example about 50 liters per m2 of processed material. Even in the device with the partial circuit described above, the amount of wastewater is still so large that a complete cleaning and desilvering before discharge into the sewage system would be too expensive for practice.
  • gelatin in particular is present in the wash-out water in dissolved form and therefore cannot be separated off by filtration. But even the dispersed pigment with a particle size far below 1 ⁇ m can only be removed using very fine filters. If you wanted to design such a fine filter for the required throughput, you would get completely unacceptable dimensions.
  • the invention has for its object to provide a method for processing a light-sensitive recording material for tanning development, in which the waste water is largely free of silver and other components of the recording material. Another object is to provide an apparatus for performing this method.
  • the object is achieved by a method according to claim 1 and a device according to claim 10.
  • the pH of the washout liquid is preferably in the acidic range.
  • the range from 4.0 to 5.0 is particularly preferred.
  • a relatively coarse filter material can be used to separate the flakes from the remaining wash-out liquid. Depth filters are preferred because they are able to absorb a large amount of solid matter before they become clogged. Filter fleeces are suitable, for example. Of course, other filter devices, in particular automatically backwashing filters, such as are known for separating sludge from waste water, or filter centrifuges can also be used.
  • the required amounts of washout liquid can be worked up even with a limited filter area. Therefore, the entire stream of used wash-out liquid is preferably passed through the filter.
  • the filter retains practically all of the silver halide and pigment washed out of the recording layer during processing. With a suitable choice of filter material, long service lives can be achieved. The waste materials mentioned are heavily enriched in the filter material, so that their recovery or disposal is economical.
  • the recording material is preferably treated with an acidic stop bath. This treatment is done after the alkaline activator bath and before washing out.
  • the stop bath preferably contains none Silver solvents such as sodium or ammonium thiosulfate. It is thereby achieved that the undeveloped silver halide is still present as a solid even in the washout stage.
  • the used washing-out liquid is filtered and fed back to the washing-out device via a pump.
  • the entire wash-out liquid can be circulated. But you can also circulate a part, feed the rest of the sewer system and replace it with fresh water.
  • at least 90% of the wash-out liquid is circulated. If the fresh water content is low, cold tap water can be used.
  • the heat generated by the high-pressure pump is then sufficient to heat the fresh water portion to the wash-out temperature. This advantageously eliminates the need for a hot water installation.
  • foam can form during washing. This foam can contain the majority of the flakes. In this case, the foam is preferably separated from the wash-out liquid before filtering, for example by means of an overflow, with a filter centrifuge, and the filtrate is added to the circuit again.
  • the stop bath is inevitably gradually neutralized by the liquid carried along by the recording material from the alkaline activator bath. It is therefore necessary to regenerate the stop bath according to the material throughput so that pH and ionic strength are stabilized and uniform results are achieved. This is usually done by adding a fresh stop bath or a concentrate. As a result, part of the bath overflows and must be collected and disposed of.
  • the washing liquid If all or part of the washing liquid is circulated, its acidity must also be regulated. There are two opposing influences Take into account: The carryover of acidic stop baths lowers the pH, while dilution with fresh water increases it. In a preferred embodiment of the method according to the invention, the proportion of the fresh water is adjusted so that the pH of the wash-out liquid is maintained in the preferred range of 4.0 to 5.0 by the dragged stop bath alone.
  • the easiest way to regenerate the wash-out liquid is to add fresh water at some point in the circuit. This can take place, for example, in the course of the washout area or, if fresh water has sufficient pressure, in the pressure line from the pump to the washout device.
  • the pH of the acid stop bath is preferably 4.0 to 4.6.
  • it can be a sufficiently dilute, preferably weak, acid.
  • acetic acid, citric acid, formic acid, lactic acid, malic acid, tartaric acid, phosphoric acid are suitable.
  • a stop bath which is buffered is particularly preferred.
  • the result of this is that the pH value is not increased inadmissibly by an alkaline activator bath which is carried over.
  • the buffering because of the dragging of the stop bath into the washing device, the buffering also has a favorable effect on the stability of the pH value of the washing liquid.
  • the stop bath contains acetic acid and is optionally buffered with alkali acetate.
  • the overflowing wash-out liquid can still remove any residual solids before it is fed into the channel passed through a fine filter with a pore size of 5 to 30 ⁇ m.
  • a fine filter with a pore size of 5 to 30 ⁇ m.
  • This can be, for example, a candle filter, a bag filter or a flat paper filter.
  • the alkaline activator bath is also usually regenerated by adding fresh activator solution or from a concentrate in order to compensate for losses caused by the development reaction and by carryover.
  • the overflowing bath is collected and may have to be disposed of.
  • the tanning-developable recording material to be used for carrying out the method according to the invention consists of a layer support on one side of which one or more layers are arranged which contain at least uncured gelatin, a light-sensitive silver halide, a dispersed pigment and a gelatin-tanning developer substance as essential components.
  • the other side of the support can either have the same or a similar light-sensitive layer structure or a non-light-sensitive auxiliary layer, for example an anticurl or antistatic layer, or it can be uncoated.
  • the essential components mentioned can be present together in one layer. But it is also possible to spread them over several layers on one side.
  • the pigment in a first layer directly on the support, the silver halide in a second layer arranged above the first and the tanning developer substance can be contained in a third outer layer, with uncured gelatin being present as a binder in all three layers.
  • Such a layer structure is described in EP 02 03 468-B1.
  • Another distribution is also possible if it is ensured that the mass transport for the imaging processes during processing, namely the development of the exposed silver halide by the tanning developer substance and the hardening of the gelatin in the layer containing the pigment, is not hindered.
  • the layer structures described can be produced by applying dispersions which contain the pigment, the silver halide, the tanning developer substance and gelatin in each case as a binder, in succession or - with the aid of a multiple coating device - also simultaneously on the layer support and drying. If a layer is to contain several components, the dispersions are mixed before coating.
  • Non-tannable binders for example polyvinyl alcohol, are also suitable for an outer layer which does not contain the pigment.
  • the silver halide is preferably in the form of a photographic silver halide emulsion prepared by conventional methods. Such methods are described, for example, in Research Disclosure 308119 (December 1989). Emulsions of silver chloride, silver bromide and silver iodide as well as those containing mixed crystals of these components or mixtures of such emulsions can be used. Silver chloride, silver bromide and silver chlorobromide are preferred.
  • the emulsions can be coarse or fine-grained; a preferred range of the average grain size is between 0.1 and 0.7 ⁇ m.
  • the uncured gelatin contained in the silver halide-containing layer and possibly in auxiliary layers is preferably an alkaline digested quality. Bone gelatin is particularly preferred.
  • the silver halide emulsions can be prepared by precipitation using the single-jet or double-jet method, if appropriate also with regulation of the pAg value.
  • Their microcrystals can be irregularly limited or, for example, also have the shape of cubes, octahedra, tetradecahedra or even flat plates.
  • Emulsions in which the soluble salts were removed by known methods after the precipitation are preferred.
  • the flock process is preferably used, in which the emulsion contains an acidic polyelectrolyte, for example according to US Pat. No. 2,772,165, or an acidic gelatin modified, for example with succinic or phthalic anhydride, and is adjusted to an acidic pH after the precipitation of the silver halide .
  • the emulsion flakes thus obtained are washed with water or dilute acid and then redispersed by adjusting a neutral or weakly alkaline pH, if appropriate in the presence of additional gelatin.
  • the emulsions are preferably chemically ripened, for example by digestion in the presence of sulfur compounds, noble metal salts and / or reducing agents. They can be sensitized for certain spectral ranges at any point in the production by adding known dyes.
  • the amount of the silver halide emulsion is preferably selected so that the silver content of the light-sensitive material is between 0.3 and 3 g per m2.
  • the layers of the light-sensitive recording material can also contain other polymeric or high-molecular substances. These can be water-soluble or, if they are not water-soluble, can be present as a dispersion. Examples are dextran, polyvinyl alcohol, latices made from polyacrylates, if appropriate with functional groups such as carboxylic acid groups or quaternary ammonium groups.
  • tanning developer substances substances are referred to here which on the one hand act as developers with respect to exposed silver halide, and on the other hand form substances in the course of the development reaction which crosslink the gelatin and thereby make it insoluble. All substances known with this property can be used. Examples are hydroquinone and in particular its diffusion-hindered derivatives, for example according to EP 01 05 108-B1, pyrogallol and its derivatives, pyrocatechol and its derivatives and polyhydroxy-spiro-bis-indane according to US 34 40 049.
  • tanning developer substances are not water-soluble in a neutral environment.
  • such substances can either be dissolved in a high-boiling solvent or finely ground in a known manner and dispersed in water with a suitable wetting agent or in the aqueous solution of a suitable hydrophilic binder.
  • the amount of the tanning developer substance is determined, inter alia, according to the amount of silver halide present and is preferably 0.5 to 5 gram equivalent per mole of silver halide.
  • the tanning developer substance is preferably incorporated into the outer layer of the recording material.
  • this layer can also contain a non-tannable binder, for example polyvinyl alcohol.
  • Water-insoluble pigments are preferably used as coloring components. They must not adversely affect the silver halide emulsion, for example by obscuring, desensitizing or tanning the gelatin. If necessary, this can be done by a Pretreat with hydrophilic binders, wetting agents and the like, for example according to DE 28 32 530-C2.
  • Organic pigments are suitable, e.g. Phthalocyanine, quinacridone and dioxazine pigments.
  • carbon black or metallic silver can be used for black images. Gas or furnace blacks are preferred.
  • the device for processing the tanning-developable light-sensitive material consists of the treatment stations activator or development tank 1 , tank for the acid bath 2 and washing device 3 . There is also a transport device which feeds the recording material to be processed into the device, feeds and outputs it through the individual stations.
  • This transport device is formed in a manner known per se from transport rollers 4 and guide plates 5 and from a conveyor belt 6 .
  • a dryer not shown here, can also be present as the fourth treatment station after the washing device.
  • the activator tank 1 contains the alkaline activator bath 7 , the level of which is limited by an overflow 8 .
  • the tank 2 contains the acid bath 9 , which can overflow through the overflow 10 .
  • Devices for the regeneration of the Activator baths and acid baths, which convey the regenerate solutions into tanks 1 , 2 are also provided, but are not shown here for the sake of simplicity.
  • Transport rollers 4 and baffles 5 convey the recording material in the tanks 1 , 2 in each case on a U-shaped path through the baths. The recording material is fed through the opening 11 into the tank 1, transferred through the opening 12 in the tank 2, and finally transported through the opening 13 in the Auswasch disposer. 3
  • the wash-out device includes both the wash-out container 3 with the conveyor belt 6 and the spray pipes 14 and also the devices for conveying, preparing and disposing of the wash-out liquid.
  • the wash-out container 3 has an outlet 15 at its lowest point, which leads the wash-out liquid which flows out after the wash-out directly to a filter 16 without a sump forming.
  • the filter 16 is connected to a buffer vessel 17 on its output side.
  • the filter and buffer vessel are preferably arranged under the washout tank, so that the washout liquid 18 reaches the buffer vessel 17 solely by gravity through the filter 16 .
  • a pump 19 is inserted into a delivery line 20 , which leads from the buffer vessel 17 to the spray pipes 14 . This closes the washing liquid circuit.
  • Fresh water for regenerating the wash-out liquid can be metered into the wash-out tank 3 through an inlet 21 .
  • the buffer vessel 17 is also provided with an overflow 22 through which the excess wash-out liquid which occurs as a result of the regeneration can flow off.
  • the filter 116 is integrated into the buffer vessel 117 . It then forms a largely horizontal one Area that separates an upper part 123 of the buffer vessel from a lower part 124 .
  • the lower part 124 is provided with a drain 120 which is connected to the high pressure pump (19).
  • the supply of washout liquid 118 in the buffer vessel is so large that it not only fills the lower part 124 but also partially the upper part 123 of the buffer vessel 117 .
  • the filter 116 is therefore preferably in a horizontal plane between the bottom of the buffer vessel and the highest possible liquid level and thus separates a portion of unfiltered washout liquid in the upper part of the buffer vessel from a filtered portion in the lower part.
  • a depth filter in particular a filter fleece with a thickness of 0.5 to 5 cm and a weight per unit area of 50 to 500 g / m 2, is preferably used as the filter.
  • the pore size must correspond to the size of the flakes, but also allow sufficient throughput.
  • the filter fleece is supported in a known manner, for example by a sieve or a perforated plate, which are not shown here. It can consist, for example, of cellulose, polyethylene, polypropylene, polycarbonate, polyester or mineral fibers.
  • filters made of combustible material preferably viscose.
  • the buffer vessel is preferably provided with an overflow 122 .
  • a weir 125 is provided. When the washing device is at a standstill, the entire washing liquid 118 collects in the buffer vessel. An excess of the intended filling volume then flows through the overflow 122 .
  • the overflow 122 of the buffer vessel 117 is particularly preferably still connected to a fine filter 126 .
  • a fine filter 126 This can be, for example, a paper or candle filter with an average pore size of approximately 5 to 30 ⁇ m.
  • the foam formation in the wash-out stage is significantly less than in the processes according to the prior art. This may be due to the fact that the foam-forming components of the washed-off recording layer are bound in the flakes and are not freely dissolved in the water. It is therefore possible to dispense with the usual addition of antifoams to the washout liquid. It is also advantageous that the washed-out pigments are removed almost completely from the washing device and do not lead to annoying soiling.
  • the process according to the invention has a significantly reduced need for warm fresh water compared to the prior art and enables considerable savings in water and energy.
  • the costs for the provision and disposal of a fixing bath are eliminated.
  • the object of the invention can be used in the production of pigmented relief images from gelatin-containing layers. Such images are used for example in reproduction in the printing industry as line and raster images and in color inspection processes in prepress.
  • the amounts of the emulsion constituents are based on 1 mol of silver halide, unless stated otherwise.
  • This dispersion was stirred into a solution of 100 g of alkaline digested bone gelatin and 2 g of sodium lauryl sulfonate in 1100 ml of water and 40 g of an aqueous dispersion of an acrylic acid-acrylate copolymer with a solids content of 40% by weight were added.
  • the application weight of this layer was such that an optical density of 3.0 resulted after drying.
  • Middle layer A silver chlorobromide emulsion with 30 mole percent bromide, a gelatin content of 20 g and an average grain size of 0.4 ⁇ m was produced using the double-jet process with pAg control. After the soluble salts had been removed by means of the flocking process according to US Pat. No. 2,772,165, the flocked emulsion was redispersed with a further 50 g of gelatin and subjected to sulfur-gold ripening. An optical sensitizer was then added and stabilized with 0.7 g of 5-hydroxy-7-methyltetrazainden.
  • Example 1 The recording material described in Example 1 was exposed as described there.
  • the processing was carried out by activating for 10 s with an activator bath of the composition given in Example 1 and washing out with the wash-out liquid AW or BW, i.e. H. without acid bath. After filtering through a paper filter, the wash-out liquid AW was still black, BW was colorless.
  • Example 1 The recording material produced and exposed as described in Example 1 was processed in a device according to FIG. 1, but with a filter integrated in the buffer vessel according to FIG. 2, at a throughput speed of 150 cm / min with a material width of 60 cm.
  • the processing conditions were the same as for Sample 4 of Example 1, but the washing liquid was circulated. 0.5 l of cold tap water was fed into the circuit per minute; about the same amount ran as Waste water from the buffer vessel.
  • the high pressure pump for the washing liquid circuit delivered 50 l / min.
  • a filter fleece with an area of 0.07 m2, a thickness of 2 cm and a basis weight of 200 g / m2 served as the filter.
  • the pH of the wash-out liquid was still 4.7.
  • the silver content of the wastewater was less than 0.1 mg / l.

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  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Silver Salt Photography Or Processing Solution Therefor (AREA)
EP93114390A 1992-09-28 1993-09-08 Verfahren und Vorrichtung zur Verarbeitung eines lichtempfindlichen Aufzeichnungsmaterials für gerbende Entwicklung Withdrawn EP0590364A2 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE4232452 1992-09-28
DE19924232452 DE4232452A1 (de) 1992-09-28 1992-09-28 Verfahren und Vorrichtung zur Verarbeitung eines lichtempfindlichen Aufzeichnungsmaterials für gerbende Entwicklung

Publications (2)

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EP0590364A2 true EP0590364A2 (de) 1994-04-06
EP0590364A3 EP0590364A3 (enrdf_load_stackoverflow) 1994-08-31

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EP93114390A Withdrawn EP0590364A2 (de) 1992-09-28 1993-09-08 Verfahren und Vorrichtung zur Verarbeitung eines lichtempfindlichen Aufzeichnungsmaterials für gerbende Entwicklung

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EP (1) EP0590364A2 (enrdf_load_stackoverflow)
DE (1) DE4232452A1 (enrdf_load_stackoverflow)

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2832530C2 (de) * 1978-07-25 1984-08-02 Du Pont de Nemours (Deutschland) GmbH, 4000 Düsseldorf Lichtempfindliches Material für die Gerbentwicklung
US4279644A (en) * 1980-06-06 1981-07-21 E. I. Du Pont De Nemours And Company Recovery of silver from photographic processor effluents
EP0181968A1 (en) * 1984-11-20 1986-05-28 Agfa-Gevaert N.V. Process for the production of photographic relief images by tanning development and wash-off processing of silver halide emulsion materials

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DE4232452A1 (de) 1994-03-31

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