WO1985002690A1 - Procede d'utilisation de liquides et de films photographiques uses - Google Patents

Procede d'utilisation de liquides et de films photographiques uses Download PDF

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Publication number
WO1985002690A1
WO1985002690A1 PCT/DE1984/000274 DE8400274W WO8502690A1 WO 1985002690 A1 WO1985002690 A1 WO 1985002690A1 DE 8400274 W DE8400274 W DE 8400274W WO 8502690 A1 WO8502690 A1 WO 8502690A1
Authority
WO
WIPO (PCT)
Prior art keywords
silver
exposed
baths
films
salt solution
Prior art date
Application number
PCT/DE1984/000274
Other languages
German (de)
English (en)
Inventor
Rainer Bojarski
Hans-Joachim GÜNTHER
Kurt Herbst
Wilhelm Stadler
Kurt Fischer
Original Assignee
Fischer Recycling Gmbh U. Co. Kg
Firma Stadler
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
Application filed by Fischer Recycling Gmbh U. Co. Kg, Firma Stadler filed Critical Fischer Recycling Gmbh U. Co. Kg
Publication of WO1985002690A1 publication Critical patent/WO1985002690A1/fr

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/72—Treatment of water, waste water, or sewage by oxidation
    • C02F1/722—Oxidation by peroxides
    • 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
    • G03C11/00—Auxiliary processes in photography
    • G03C11/24—Removing emulsion from waste photographic material; Recovery of photosensitive or other substances
    • 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
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
    • C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
    • C02F2103/40—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32 from the manufacture or use of photosensitive materials

Definitions

  • the invention relates to a method for the combined recovery and disposal of used exposed, developed and exposed and undeveloped films and photo papers, as well as pollutants in photochemical waste liquids, and the recovery of the plastic carrier material.
  • Wastewater is currently undergoing electrolysis treatment to separate the silver content, which is then melted and returned to the industry.
  • the object of the present invention is to propose a method which includes the disposal and chemical recycling for waste and pollutants from the photo-chemistry as a whole.
  • the invention a large number of different materials are processed, some of which are known per se, but the resulting liquids are subjected to a common utilization.
  • the invention is seen in particular in the combination of the individual process steps, which leads to a complete disposal of the resulting substances.
  • the method according to the invention provides for the utilization of exposed and developed film and photo paper 10 via the feed line 11, of exposed or unexposed but not developed film material and photo paper 12 via the line 13, and silver-containing fixing liquid 14 via the line 15.
  • Photographic developers 16 are also used via line 17 and further photochemical waste water 18 such as activator liquids, stop baths, cyanide solutions, nitrite solutions, etc., via line 19.
  • the silver is in the elemental state as Ag ° and can no longer be dissolved in Na 2 S 2 O 3 / (NH 4 ) 2 S 2 O 3 solution.
  • the enclosing gelatin layer must be opened up.
  • the delivered material 10 is first sorted by format and fed to a shredding device 19, in particular a face cutter, which cuts strips of 6 ⁇ 2 cm at a height of 10 cm in two work steps. The cut material is fed to a high depot 20 and from there to a washing device 21.
  • a solution which is suitable for swelling and hydrolling the gelatin is added to this washing device via a line 22.
  • This can be done with hydrochloric acid as well as with biocatalysts.
  • bacterial proteinase enzymes are preferably used, since they carry out hydrolytic cleavage of the gelatin in a natural process and are therefore environmentally friendly.
  • the gelatin in D- and L-form of the proline and of the hydroxiproline is split by the ferments at a temperature of approximately 40 ° and a neutral pH.
  • the fission products mentioned are soluble in water, as a result of which the gelatin releases the elemental silver.
  • This finely divided silver is present as a stabilized colloid, and the colloidal solution is used again for further concentration for washing off.
  • the film material washed off in this way is then in the form of a pure plastic material and is removed from the enzyme reactor 21 via the line 23 and is recycled as a recyclable plastic 24, ie. H. fed to industry.
  • the first raw material is thus recovered.
  • photo paper which is also recovered (36).
  • the enzyme solution is concentrated to such an extent that it is used up.
  • the protective colloid formed must be destroyed in order to obtain the colloidally distributed silver. This is preferably achieved by lowering the pH. For this the liquid is transported into a precipitation container 25 and the pH is reduced from seven to four by adding sulfuric acid via line 26. This causes the colloid to collapse and the small particles to form larger aggregates. The coagulation leads to the immediate onset of sedimentation.
  • the resulting dispersion is separated into solid 28 and liquid phase 29.
  • the process waste water in the silver content is below 1 g / m 3 , while the COD value, ie the chemical oxygen demand, is approx. 5,000 mg O 2 / ltr. is.
  • This wastewater is post-treated in a special wastewater treatment plant 30 to adapt the chemical oxygen.
  • the solid 28 discharged from the decanter consists of a mixture of silver and non-split gelatin and is subjected to a thermal treatment stage 31 at 1,100 ° C. in order to melt the crude silver.
  • a thermal treatment stage 31 at 1,100 ° C. in order to melt the crude silver.
  • borax as a melting agent, the silver is obtained as a raw silver ingot 32 and thus the second recycling product.
  • Exposed or unexposed but undeveloped film material and photographic paper 12 are fed via line 13 to the system described above as a further material to be treated in a separate work process.
  • This material is used in the production of films and photo paper and consists of sections, roll end pieces and rejects.
  • the silver bromide applied in the photographic emulsion remains unchanged on this material, or by exposure in the activated form Ag * Br, since the material has not yet come into contact with the reducing hydroquinone of the developer. However, it can be completely dissolved with fixation salt solution.
  • the method according to the invention provides that this material is first treated in the same way as the exposed and already developed material to be used.
  • the shredding device 19 which can also be a shredder, shredded and eluted in the washing device 21 by means of a Na 2 S 2 O 3 / (NH 4 ) 2 S 2 O 3 solution, the Dissolving process is accelerated by stirring.
  • this washing process can be carried out in a separate washing container, not shown in the figure, provided that the washing device 21 is constantly required as an enzyme reactor.
  • the eluate obtained by this washing process has silver ions bound as a silver thionate complex and is fed via line 33 to an electrolysis device in order to recover the silver. After the electrolysis, the eluate still has a residual content of approx. 1 g / ltr. and is to be used again for washing newly prepared material. This return line is indicated at 35 in the figure. After the washout has taken place, the carrier material is fed via line 23 to the plastic recycling 24 or the paper recovery 36.
  • the washing device 21 therefore serves as a combined device for the utilization of exposed and developed or exposed or unexposed, but not developed film material and photo paper.
  • the former is processed via an enzyme treatment, the latter using a fixing salt solution in order to obtain the raw materials plastic or paper.
  • the silver contained is then recovered either via the precipitation process with subsequent thermal treatment (stages 25, 31) or via the electrolysis device 34.
  • the method according to the invention further provides that silver-containing fixing liquid 14 is disposed of. Fixing liquid containing silver is formed in the photographic process if non-activated silver bromide is removed from the gelatin layer by fixing after the development process. This liquid is fed via line 15 to the electrolysis device 34, where the silver is deposited cathodically. The silver obtained in this way is then melted in melting furnace 37 at 1,100 ° C. to form crude silver bars 32.
  • the used desilvered fixing salt solution has a COD value, ie a chemical oxygen demand of over 100,000 mg O 2 / ltr. and must therefore be subjected to wastewater treatment.
  • the liquid is fed via line 38 to the wastewater treatment plant 30.
  • Another used photo-chemical material is used to remove photographic developer 16, which consists of an alkaline, aqueous solution which contains hydroquinone, phenylenediamine and pheniodone, and also sulfites, soda and borax.
  • the COD value is also over 100,000 mg O 2 / ltr.
  • the developer is consumed by the oxidation of the hydroquinone and turns red-brown. This liquid is also fed via line 17 to the wastewater treatment plant 30 for further processing.
  • the process according to the invention also allows further photo-chemical liquids 18, such as activator liquids, stop baths, cyanite solutions, and nitrite solutions, to be used.
  • the alkaline oxidation also takes place in the wastewater treatment plant 30, for which purpose detoxification takes place immediately.
  • Such liquids must not come into contact with acid, as this produces life-threatening vapors.
  • the wastewater treatment plant 30 must be regarded as the centerpiece of the invention, since all the photo-chemical liquids which arise or are present in the process are subjected to a final treatment here.
  • the fixing liquid electrolytically desilvered via line 38 also contains thiosulfates, sulfites, sulfides and sulfates, and also the
  • the developer liquid 16 supplied via line 17 to the wastewater treatment plant 30 is slightly alkaline and contains organic compounds such as phenols, hydroquinone, formaldehyde, etc.
  • Both liquids ie the desilvered fixing salt solution and the developer solution, are subjected to catalytic oxidation in the fully automatic wastewater treatment plant 30, ie all oxygen-consuming compounds are oxidized and thus converted into a stable oxidation state.
  • All thiosulfate ions are oxidized to the sulfate and precipitated in the presence of CA (OH) 2 or Ba (OH) 2 as Ca SO 4 or Ba SO 4 . After precipitation, they are removed from the process using a floating filter and can be used industrially as gypsum or white pigment. Since the filtrate still contains NH 4 + ions, it is subjected to stripping. The NH 3 is thus removed from the solution.
  • the COD value reduction by approx. 90,000 to less than 10,000 mg O 2 / ltr. is reproducible and is achieved with every batch.
  • the organic components of the developer liquid 16 such as phenols, hydroquinone and formaldehyde, are converted by the catalytic oxidation into carboxylic acid or dicarboxylic acids, all of which are biodegradable.
  • the entire residual liquid of the wastewater treatment plant can therefore be transferred to the sewage system 39 and from there to conventional municipal wastewater treatment plants 40.
  • the process wastewater has a neutral pH of 7 and an approved COD of less than 10,000 mg O 2 / ltr. and can thus be led directly into the sewage system.
  • the process wastewater can be degraded without damaging the bacterial flora in a biological sewage treatment plant.
  • the process scheme set out below shows in detail the processes of liquid treatment and detoxification of the fixing salt solution and of the developer solution in the wastewater treatment plant 30.
  • the clear remaining process liquid finally only contains sulfate ions (approx. 1,000 mg / l) of ammonium ions, as well as organic compounds from the developer liquid.
  • sulfate ions approximately 1,000 mg / l
  • the ammonium concentration can be reduced further by raising the pH to twelve and removing the ammonia by blowing in air or converting the ammonia to N 2 by catalytic oxidation.
  • the system is oxidized again to make a pH correction and the treated liquid is slowly (approx. 200 - 400 ltr./h) metered into the sewage system.
  • An ion exchange and an activated carbon adsorption stage are provided as the standby system for the polishing functions.
  • the analytical information before and after the treatment of the photo-chemical liquids in the wastewater treatment plant can be presented as follows:
  • COD 200,000 mg O 2 / ltr. COD: 200 mg - 10,000 mg O 2 / ltr.
  • the residual liquid from the decanter 27, which is also to be degraded in the wastewater treatment plant 30, contains L-proline and L-hydroxiproline after the gelatin has been fermented.
  • the addition of sulfuric acid to the precipitation of acidic liquid contains 30 hydrolidin-2-carboxylic acid, hydroxiproline, and 4-hydroxipyrolidin-2-carboxylic acid, all of which are biodegradable, which means that this fermented wastewater can be safely discharged into the Sewerage 39 is possible.
  • the support of the biological clarification stage by the biocatalysts in the process wastewater may even be a desirable phenomenon.
  • the system configuration described above combines the entire recycling and elimination of pollutants of all substances occurring in the photo-chemical industry.
  • the procedure has been checked and approved with regard to the requirements of water management authorities, so that the procedure is directly applicable in practice.

Landscapes

  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Removal Of Specific Substances (AREA)
  • Silver Salt Photography Or Processing Solution Therefor (AREA)
  • Water Treatment By Electricity Or Magnetism (AREA)

Abstract

Procédé servant à la fois à l'utilisation et à l'élimination de tous les matériaux engagés lors du traitement photochimique des films. Il permet la récupération de l'argent, du plastique et du papier. Les films exposés et développés sont soumis à un traitement enzymatique, l'argent contenu dans la gélatine étant récupéré grâce à un processus thermique. La solution de sel fixatif désargentée au cours d'un traitement électrolytique est amenée, de concert avec la solution de révélateur, les eaux usées du matériau de film traité enzymatiquement et les autres liquides photochimiques, à une installation commune de purification des eaux usées pour y subir une oxydation catalytique. L'eau industrielle ainsi obtenue peut être amenée sans autre aux égouts et à une installation d'épuration biologique.
PCT/DE1984/000274 1983-12-15 1984-12-14 Procede d'utilisation de liquides et de films photographiques uses WO1985002690A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DEP3345346.2 1983-12-15
DE19833345346 DE3345346A1 (de) 1983-12-15 1983-12-15 Verfahren zur verwertung von verbrauchten photografischen filmen und fluessigkeiten

Publications (1)

Publication Number Publication Date
WO1985002690A1 true WO1985002690A1 (fr) 1985-06-20

Family

ID=6216981

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/DE1984/000274 WO1985002690A1 (fr) 1983-12-15 1984-12-14 Procede d'utilisation de liquides et de films photographiques uses

Country Status (3)

Country Link
EP (1) EP0165269A1 (fr)
DE (1) DE3345346A1 (fr)
WO (1) WO1985002690A1 (fr)

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0238148A1 (fr) * 1986-03-20 1987-09-23 Paques B.V. Procédé pour la purification d'eau usée
WO1991016667A1 (fr) * 1990-04-19 1991-10-31 Devappa Dr. Ing. R. Zinsser & Ing. K. Prestl Installation de developpement pour bases d'emulsions photographiques
WO1992004660A1 (fr) * 1990-09-07 1992-03-19 Kodak Limited Procede de traitement d'effluents
WO1992011208A1 (fr) * 1990-12-18 1992-07-09 Kodak Limited Procede de traitement d'effluents
FR2688777A1 (fr) * 1992-03-19 1993-09-24 Kodak Pathe Procede de traitement d'effluents liquides contenant des composes organiques.
US5326477A (en) * 1990-05-07 1994-07-05 Bio-Sep, Inc. Process for digesting solid waste
EP0861810A2 (fr) * 1997-02-28 1998-09-02 Eastman Kodak Company Méthode pour le traitement des résidus liquides de procédés photographiques
EP0861807A2 (fr) * 1997-02-28 1998-09-02 Eastman Kodak Company Méthode de traitement des résidus liquides de procédés photographiques

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE4031609A1 (de) * 1990-03-16 1991-09-19 Kodak Ag Verfahren und vorrichtung zur aufbereitung von fluessigen rueckstaenden aus photographischen prozessen
DE4105368C1 (en) * 1991-02-21 1992-05-07 Papierfabrik Schoellershammer Heinr. Aug. Schoeller Soehne Gmbh & Co Kg, 5160 Dueren, De Handling photographic paper having plastic coating - includes dissolving cellular material from plastic using strong base
DE19829274C2 (de) * 1998-07-01 2002-06-20 Otb Oberflaechentechnik Berlin Verfahren zur Rückgewinnung von Edelmetallen

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Publication number Priority date Publication date Assignee Title
DE2009826A1 (en) * 1970-03-03 1972-01-27 Degussa Hydrogen peroxide - for developer, clarifying and fixing bath detoxication and silver recovery
EP0022526A1 (fr) * 1979-07-11 1981-01-21 Bayer Ag Procédé de traitement d'eaux résiduaires
US4299676A (en) * 1980-01-31 1981-11-10 Photographic Silver Recovery Limited Recovery of silver from photographic film
US4332687A (en) * 1978-09-21 1982-06-01 Pca International, Inc. Removal of complexed heavy metals from waste effluents
FR2534900A1 (fr) * 1982-10-20 1984-04-27 Rehman Process Eng Procede de traitement des solutions de travail des industries photochimiques

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US3733256A (en) * 1970-10-12 1973-05-15 Future Systems Inc Process for extracting silver from silver bearing materials
US3982932A (en) * 1972-08-22 1976-09-28 Eastman Kodak Company Recovery of silver from gelatinous photographic wastes
US3961976A (en) * 1974-05-17 1976-06-08 Sca Development Aktiebolag Method of preparing size
DE2430848C2 (de) * 1974-06-27 1986-02-27 Levrini, Valter, Castellarano Verfahren zur chemischen Reinigung von Abwässern
US3954594A (en) * 1974-09-04 1976-05-04 Rockwell International Corporation Electrochemical cell for decreasing the cyanide and heavy metal content of an aqueous solution
NL7604579A (nl) * 1975-04-30 1976-11-02 Westinghouse Electric Corp Werkwijze en inrichting voor het verwijderen van verontreinigingen uit water.
IT1065003B (it) * 1976-03-23 1985-02-25 Anic Spa Procedimento per il recupero di elementi a valenza variabile da acque di scarico contenenti loro composti e depurazione delle acque stesse
DE2719667C2 (de) * 1977-05-03 1986-09-11 GOEMA, Dr. Götzelmann KG, Physikalisch-chemische Prozeßtechnik, 7000 Stuttgart Vorrichtung zur Behandlung von metallhaltigem Abwasser
DE2724724C3 (de) * 1977-06-01 1982-12-16 Nihon Filter Co. Ltd., Tokyo Verfahren und Anlage zum Aufbereiten von schwermetallhaltigen Abwässern unter Rückgewinnung von Schwermetallen
JPS561049A (en) * 1979-06-15 1981-01-08 Fuji Photo Film Co Ltd Regenerating method for waste photographic processing solution
JPS561048A (en) * 1979-06-15 1981-01-08 Fuji Photo Film Co Ltd Regenerating method for waste photographic processing solution
DE3009449A1 (de) * 1980-03-12 1981-09-24 Photographic Silver Recovery Ltd., Waltham Cross, Hertfordshire Verfahren und vorrichtung zur wiedergewinnung von silber aus fotografischem material

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2009826A1 (en) * 1970-03-03 1972-01-27 Degussa Hydrogen peroxide - for developer, clarifying and fixing bath detoxication and silver recovery
US4332687A (en) * 1978-09-21 1982-06-01 Pca International, Inc. Removal of complexed heavy metals from waste effluents
EP0022526A1 (fr) * 1979-07-11 1981-01-21 Bayer Ag Procédé de traitement d'eaux résiduaires
US4299676A (en) * 1980-01-31 1981-11-10 Photographic Silver Recovery Limited Recovery of silver from photographic film
FR2534900A1 (fr) * 1982-10-20 1984-04-27 Rehman Process Eng Procede de traitement des solutions de travail des industries photochimiques

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* Cited by examiner, † Cited by third party
Title
Chemistry and Industry, No 14, July 1983, London (GB) A.F.E. Sims: "Industrial Effluent Treatment with Hydrogen Peroxide", pages 555-558, see pages 556, 557 *
Research Disclosure, No 160, August 1977, Homewell, Havant, Hampshire (GB) "Ein Neues Verfahren zur Oxidation Photpgraphischer Abwasser", pages 38, 39, see page 38, 39 *

Cited By (16)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4765901A (en) * 1986-03-20 1988-08-23 Pacques B.V. Method for purifying waste water
EP0238148A1 (fr) * 1986-03-20 1987-09-23 Paques B.V. Procédé pour la purification d'eau usée
WO1991016667A1 (fr) * 1990-04-19 1991-10-31 Devappa Dr. Ing. R. Zinsser & Ing. K. Prestl Installation de developpement pour bases d'emulsions photographiques
US5326477A (en) * 1990-05-07 1994-07-05 Bio-Sep, Inc. Process for digesting solid waste
US5709796A (en) * 1990-05-07 1998-01-20 Bio-Sep, Inc. Process for digesting cellulose containing solid wastes
WO1992004660A1 (fr) * 1990-09-07 1992-03-19 Kodak Limited Procede de traitement d'effluents
US5350522A (en) * 1990-09-07 1994-09-27 Eastman Kodak Company Effluent treatment
WO1992011208A1 (fr) * 1990-12-18 1992-07-09 Kodak Limited Procede de traitement d'effluents
US5419840A (en) * 1990-12-18 1995-05-30 Eastman Kodak Company Effluent treatment
WO1993019011A1 (fr) * 1992-03-19 1993-09-30 Kodak-Pathe Procede de traitement d'effluents liquides contenant des composes organiques
US5451324A (en) * 1992-03-19 1995-09-19 Eastman Kodak Company Method of treating liquid effluents containing organic compounds
FR2688777A1 (fr) * 1992-03-19 1993-09-24 Kodak Pathe Procede de traitement d'effluents liquides contenant des composes organiques.
EP0861810A2 (fr) * 1997-02-28 1998-09-02 Eastman Kodak Company Méthode pour le traitement des résidus liquides de procédés photographiques
EP0861807A2 (fr) * 1997-02-28 1998-09-02 Eastman Kodak Company Méthode de traitement des résidus liquides de procédés photographiques
EP0861810A3 (fr) * 1997-02-28 1998-12-02 Eastman Kodak Company Méthode pour le traitement des résidus liquides de procédés photographiques
EP0861807A3 (fr) * 1997-02-28 1998-12-02 Eastman Kodak Company Méthode de traitement des résidus liquides de procédés photographiques

Also Published As

Publication number Publication date
DE3345346A1 (de) 1985-06-27
EP0165269A1 (fr) 1985-12-27

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