EP0035008B1 - Verfahren und Apparat zur Aufbereitung photographischer Lösungen - Google Patents

Verfahren und Apparat zur Aufbereitung photographischer Lösungen Download PDF

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Publication number
EP0035008B1
EP0035008B1 EP81870013A EP81870013A EP0035008B1 EP 0035008 B1 EP0035008 B1 EP 0035008B1 EP 81870013 A EP81870013 A EP 81870013A EP 81870013 A EP81870013 A EP 81870013A EP 0035008 B1 EP0035008 B1 EP 0035008B1
Authority
EP
European Patent Office
Prior art keywords
control electrode
potential
cathode
bath
electrolysis
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
Application number
EP81870013A
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English (en)
French (fr)
Other versions
EP0035008A3 (en
EP0035008A2 (de
Inventor
Pierre F. Vandenput
Philippe A. De Meester
Jean-Pierre J. Heraly
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.)
Esterol AG
Original Assignee
Esterol AG
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Filing date
Publication date
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Application filed by Esterol AG filed Critical Esterol AG
Priority to AT81870013T priority Critical patent/ATE11602T1/de
Publication of EP0035008A2 publication Critical patent/EP0035008A2/de
Publication of EP0035008A3 publication Critical patent/EP0035008A3/fr
Application granted granted Critical
Publication of EP0035008B1 publication Critical patent/EP0035008B1/de
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Classifications

    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
    • C25C1/00—Electrolytic production, recovery or refining of metals by electrolysis of solutions
    • C25C1/20—Electrolytic production, recovery or refining of metals by electrolysis of solutions of noble metals
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
    • C25C7/00—Constructional parts, or assemblies thereof, of cells; Servicing or operating of cells
    • C25C7/06—Operating or servicing
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D21/00—Processes for servicing or operating cells for electrolytic coating
    • C25D21/12—Process control or regulation
    • 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
    • G03C5/3954—Electrical methods, e.g. electroytic silver recovery, electrodialysis
    • G—PHYSICS
    • G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03D—APPARATUS FOR PROCESSING EXPOSED PHOTOGRAPHIC MATERIALS; ACCESSORIES THEREFOR
    • G03D3/00—Liquid processing apparatus involving immersion; Washing apparatus involving immersion
    • G03D3/02—Details of liquid circulation
    • G03D3/06—Liquid supply; Liquid circulation outside tanks
    • G03D3/065—Liquid supply; Liquid circulation outside tanks replenishment or recovery apparatus

Definitions

  • the present invention relates to a method and an apparatus for the treatment of a photographic fixative bath, with a view to extracting the silver in the form of metallic silver by electrolysis in a bath comprising electrodes, it is ie at least one cathode and anodes.
  • a method and an apparatus are known in which a fixer bath is subjected to electrolysis in order to recover the silver in metallic form on at least one cathode.
  • the electric electrolysis current must have a sufficiently low intensity so that the sulfurization of the silver is avoided. Due to the fact that the electrolysis current must be low, the recovery of the silver is far from complete and it sometimes happens that more than 2 grams / liter of silver is lost in the fixing baths sent to the after their electrolysis. This obviously results in a significant loss of money economically.
  • the photographic fixer bath containing an excess of antioxidant agent is subjected to an electrolysis so as to ensure the deposition metallic silver on at least one cathode placed between two anodes in the electrolytic bath, subjected to turbulence, the pH being maintained at approximately 3.5 to 4.5 and the electrolysis current being subjected in this bath to regulation as a function of its silver content, the intensity of the current being caused to decrease as the silver content of the bath decreases.
  • the electrolysed bath can be used again as a photographic fixative bath.
  • the potential difference to be applied to the electrodes during electrolysis must include at least the potential difference to overcome the ohmic resistance of the electrolysis cell, the concentration bias due to the concentration gradients in the electrolyte and the overvoltage. inherent in the rate of reactions occurring at the electrodes.
  • the electrolysis rate is linked to the electrolysis current and therefore to the potential difference applied to the electrodes.
  • the electrolysis current is modified during the operation.
  • Apparatuses for treating photographic fixer baths are known in which the electric electrolysis current is adjusted during electrolysis, either as a function of the silver concentration of the photographic fixer bath, or as a function of the resistivity of the electrolysis cell, or again depending on the overvoltage at the cathode.
  • the state of the prior art is illustrated for example by the publication DE-B-1 187 806. These known devices have the following drawbacks.
  • Known devices based on the measurement of the overvoltage at the cathode use a reference electrode connected by a bridge of silver nitrate placed in the vicinity of the cathode and make it possible to control the electrolysis up to very low silver concentrations.
  • This system however involves the obligation to use a set of liquid junctions of different electrolytes, such as silver nitrate and for example mercury chloride, when using a calomel reference electrode.
  • the migration of different ions causes, during electrolysis, irreversible phenomena which modify the value of the overvoltage at the electrolyte junctions.
  • the present invention aims to remedy the drawbacks described above by a method of treating a photographic fixer bath in order to extract the silver in metallic form, in which the stirred photographic fixer bath containing an antioxidant is subjected. to an electrolysis so as to ensure the deposition of metallic silver on at least one cathode disposed between anodes, a control electrode being disposed near the cathode, characterized in that the intensity is adjusted electrolysis current by measuring both the resistivity of the electrolysis cell and the overvoltage at the electrodes by the potential difference between a cathode serving as a working electrode and the control electrode.
  • the invention also relates to an apparatus for treating a photographic fixer bath with a view to extracting the silver in metallic form, this apparatus comprising an electrolysis cell comprising, as electrodes, at least one cathode and anodes thus that a control electrode, characterized in that the control electrode is composed of pure carbon and is immersed in the agitated electrolytic bath near said or of a cathode serving as working electrode, and in that it comprises a regulating device connected to the control electrode and to said cathode and arranged to adjust the electrolysis current by measuring the resistivity in response to the potential difference between said control electrode and said cathode.
  • the device for regulating the electrolysis current comprises an adder assembly connected to add the potential of the control electrode and a predetermined reference potential; a comparator / integrator assembly having an input connected to the output of the adder assembly and a second input connected to receive the potential of said cathode, said assembly being arranged to integrate the potential difference between said control electrode and the reference potential and for comparing the integrated value to the potential of the cathode so as to produce a control signal, and a current generator connected to supply the electrolysis current in response to said control signal from the comparator / integrator assembly.
  • the method and the apparatus according to the invention aim to extract the silver contained in a photographic fixer bath as the silver bath becomes saturated, with a view to prolonging the duration of use of this bath.
  • the apparatus for treating a photographic fixer bath according to the invention shown in FIG. 1, comprises, in a known manner, an electrolysis cell 1 mounted downstream of an enclosure (not shown) in which s fixes a photographic film and the overflow of which is sent via a pipe 2 into the electrolysis cell 1.
  • the electrolysis cell 1 contains at least one cathode 3 in the form of a plate, for example made of stainless steel, disposed between two anodes 4 constituted, for example, by high density and high purity graphite.
  • the cathode 3 and the anodes 4 are held in place and guided in the electrolysis cell 1 by known means (not shown).
  • a device for stirring the electrolyte which may be constituted by a dip tube 5 whose upper end is bent as shown in 6.
  • This dip tube whose lower end is perforated to allow the entry of electrolyte into the tube, is connected a pipe 7 supplying this tube 5 with compressed air from a source of compressed air, not shown.
  • the compressed air supplied to the lower part of the dip tube 5 is expelled in mixture with liquid fixative through the free end 6, creating permanent agitation or turbulence in the intervals between the cathode 3 and the anodes 4, so that that the silver ions in the electrolytic bath are brought close to the cathode (s) 3 in order to be fixed there.
  • a control electrode 8 composed of pure carbon, immersed in the electrolytic bath. This electrode which has a determined potential with respect to the cathode, plays a role which will be explained later.
  • the cathode 3, the two anodes 4 and the control electrode 8 are connected by electrical conductors to a control device mounted in a housing (not shown) in which is also mounted the compressed air supply device.
  • the photographic fixative bath used in the process according to the invention is advantageously an aqueous solution containing approximately 100 to 200 g / l of ammonium or sodium thiosulfate and from 0 to 50 g / l of ammonium thiocyanate nium, as well as an excess of sodium sulfite which can reach a concentration of 60 g / l.
  • This bath also contains a known tanning agent, at a starting concentration which can reach 15 g / liter, this concentration usually being between approximately 5 and 15 g / liter.
  • the pH of the photographic fixing bath is maintained at a value of approximately 3.5 to 4.5 by adding thereto, if necessary, a small amount of an acid, such as acetic acid.
  • the electrolysis cell 1 could contain a greater number of cathodes and anodes, the number of anodes always being one unit greater than the number cathodes.
  • the electrolysis current in the electrolysis cell 1 is regulated according to the silver content of the electrolytic bath so that the current decreases when the silver content of the electrolytic bath becomes lower than a predetermined low value, for example 0.5-2 g / I.
  • a regulation device 10 illustrated diagrammatically in FIG. 2. This device is organized to maintain the potential Uec of the control electrode 8 at a predetermined set value and to compare this potential with the potential of the cathode 3 in order to regulate the electrolysis current.
  • the potential Uec of the control electrode 8 is applied by line 103 to a terminal 101 of the regulating device 10.
  • To a second terminal 102 is applied the predetermined reference or reference potential Uref.
  • the potentials Uec and Uref are of opposite polarities and are added by a resistor circuit or adder circuit 11: the sum of these potentials is applied to a first input 104 of an operational amplifier 12.
  • a second input 105 of this amplifier receives the potential Uc of the cathode 3 via the line 106 through the resistor 13.
  • An integration capacitor 14 is connected in parallel with the amplifier 12 (comparator / integrator assembly).
  • the current on the input line 104 is zero and the voltage across the terminals of capacitor 14 is at a constant value.
  • the voltage on the output line 107 of the amplifier 12 controls a current generator 15 to generate a current which, after amplification in the amplifier 16, supplies the anodes 4 to supply the electrolysis current.
  • the reference potential Uref is chosen equal to the potential that would take the control electrode 8 for a concentration of the electrolytic bath of the order of 0.5 to 2 g / I with a zero electrolysis current.
  • the reference potential Uref is for example from 300 to 600 millivolts.
  • the control electrode 8 is advantageously polarized by a low current, of 1 mA for example, to protect this electrode against damage which would be caused at the surface.
  • a low current of 1 mA for example.
  • the control electrode 8 is protected by a sheath 9, for example made of foam, to avoid turbulence of the electrolytic bath in the immediate vicinity of this electrode, such turbulence possibly having the effect of causing an undesirable variation in the potential of this electrode.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Metallurgy (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Automation & Control Theory (AREA)
  • Electrolytic Production Of Metals (AREA)
  • Silver Salt Photography Or Processing Solution Therefor (AREA)
  • Photographic Developing Apparatuses (AREA)

Claims (9)

1. Verfahren zur Behandlung eines photographischen Fixierbades zwecks Rückgewinnung von Silber als Metall, bei dem man das bewegte photographische Fixierbad, das einen Oxidationsinhibitor enthält, einer Elektrolyse derart unterwirft, daß die Silberabscheidung als Metall auf mindestens einer zwischen Anoden (4) angeordneten Kathode (3) erfolgt, wobei eine Kontrollelektrode in der Nähe der Kathode angeordnet ist, dadurch gekennzeichnet, daß man die Stärke des Elektrolysestromes einstellt, indem sowohl der Widerstand der Elektrolysezelle als auch die Überspannung an den Elektroden durch die Potentialdifferenz zwischen der als Arbeitselektrode dienenden Kathode (3) und der Kontrollelektrode (8) gemessen wird.
2. Verfahren gemäß Anspruch 1, dadurch gekennzeichnet, daß man das Potential der Kontrollelektrode (8) auf demjenigen Wert (Uref) hält, den die Elektrode hätte, falls der Silbergehalt des Elektrolysebades auf etwa 0,5 bis 2 g/I gefallen wäre, wenn der Elektrolysestrom Null beträgt.
3. Verfahren gemäß Anspruch 2, dadurch gekennzeichnet, daß man das Potential der Kontrollelektrode (8) auf einen Referenzwert von etwa 300 bis 600 Millivolt hält.
4. Verfahren gemäß einem der Ansprüche 1 bis 3, dadurch gekennzeichnet, daß man die Bewegung des elektrolytischen Bades in der Nähe der Kontrollelektrode verhindert.
5. Vorrichtung zur Behandlung eines photographischen Fixierbades zwecks . Rückgewinnung von Silber als Metall mit dem Verfahren gemäß einem der vorangehenden Ansprüche, wobei diese Vorrichtung eine Elektrolysezelle (1) enthält, welche als Elektroden mindestens eine Kathode (3) und Anoden (4) sowie eine Kontrollelektrode aufweist, dadurch gekennzeichnet, daß die Kontrollelektrode (8) aus reinem Kohlenstoff besteht und in das elektrolytische Bad getaucht ist, das in der Nähe der genannten Elektrode oder einer als Arbeitselektrode dienenden Kathode (3) bewegt ist und daß eine Einstelleinrichtung (10) vorgesehen ist, die an die Kontrollelektrode und die genannten Kathode angeschlossen und betätigt wird, um den Elektrolysestrom zu regeln, wobei der Widerstand in Abhängigkeit von der Potentialdifferenz zwischen der genannten Kontrollelektrode und der Kathode gemessen wird.
6. Vorrichtung gemäß Anspruch 5, dadurch gekennzeichnet, daß die Einstellvorrichtung (10) eine Schaltung (11-14) enthält, die die Abweichung zwischen dem Potential (Uec) der Kontrollelektrode (8) und einem vorbestimmten Referenzpotential (Uref) mißt und ein der genannten Potentialabweichung proportionales Steuersignal erzeugt derart, daß diese Abweichung auf Null reduziert und ein konstanter Wert der Potentialdifferenz zwischen der Kontrollelektrode (8) und der Kathode (3) eingehalten wird.
7. Vorrichtung gemäß einem der Ansprüche 5 und 6, dadurch gekennzeichnet, daß die Einstellvorrichtung (10) eine Additionsschaltung (11) zum Addieren des Potentials (Uec) der Kontrollelektrode (8) und eines vorbestimmten Referenzpotentials (Uref), eine Komparator/Integrator-Schaltung (12, 14) mit einem an den Ausgang der Additionsschaltung (11) angeschlossenen Eingang (104) und einem zweiten angeschlossenen Eingang (105) enthält, um das Potential der genannten Kathode (3) zu empfangen, wobei die Schaltung derart betrieben wird, daß sie die Potentialdifferenz zwischen der Kontrollelektrode und dem Referenzpotential integriert und den integrierten Wert mit dem Potential der Kathode vergleicht, so daß ein Steuersignal erzeugt wird, und daß sie einen Stromgenerator (15) umfaßt, der derart geschaltet ist, daß er den Elektrolysestrom in Abhängigkeit von dem Steuersignal der Komparator/Integrator=Schaltung (12-14) liefert.
8. Vorrichtung gemäß einem der Ansprüche 6 und 7, dadurch gekennzeichnet, daß sie eine Spannungs/Widerstands-Generatoreinrichtung (17, 18) zur Polarisierung der Kontrollelektrode (8) enthält.
9. Vorrichtung gemäß einem der Ansprüche 5 bis 8, dadurch gekennzeichnet, daß die Kontrollelektrode (8) mit einer Schutzhülle (9) versehen ist, um die Bewegung des elektrolytischen Bades in der Nähe dieser Elektrode zu vermeiden.
EP81870013A 1980-02-21 1981-02-16 Verfahren und Apparat zur Aufbereitung photographischer Lösungen Expired EP0035008B1 (de)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AT81870013T ATE11602T1 (de) 1980-02-21 1981-02-16 Verfahren und apparat zur aufbereitung photographischer loesungen.

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
LU82188A LU82188A1 (fr) 1980-02-21 1980-02-21 Procede et appareil de traitement de bains de fixateurs photographiques
LU82188 1980-02-21

Publications (3)

Publication Number Publication Date
EP0035008A2 EP0035008A2 (de) 1981-09-02
EP0035008A3 EP0035008A3 (en) 1982-06-09
EP0035008B1 true EP0035008B1 (de) 1985-01-30

Family

ID=19729355

Family Applications (1)

Application Number Title Priority Date Filing Date
EP81870013A Expired EP0035008B1 (de) 1980-02-21 1981-02-16 Verfahren und Apparat zur Aufbereitung photographischer Lösungen

Country Status (6)

Country Link
US (1) US4377456A (de)
EP (1) EP0035008B1 (de)
JP (1) JPS56138737A (de)
AT (1) ATE11602T1 (de)
DE (1) DE3168559D1 (de)
LU (1) LU82188A1 (de)

Families Citing this family (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2556374B1 (fr) * 1983-12-12 1986-08-08 Joliot Robert Dispositif pour maintenir a une valeur determinee la concentration en argent des bains de fixage dans les laboratoires cinematographiques ou photographiques
FR2582022B1 (fr) * 1985-05-14 1988-02-19 Kodak Pathe Procede et dispositif de regulation de la position du point de fonctionnement d'une cellule d'electrolyse
US4675085A (en) * 1985-07-31 1987-06-23 Adalberto Vasquez Method and apparatus for recovery of metal from solution
GB8927964D0 (en) * 1989-12-11 1990-02-14 Kodak Ltd Method and apparatus for recovering silver from a photographic fixing solution
DE69214455T2 (de) * 1992-11-10 1997-04-30 Agfa Gevaert Nv Verwendung einer pH-empfindlichen Referenz-Elektrode für die elektrolytische Entsilberung
US5770034A (en) * 1995-07-15 1998-06-23 Agfa-Gevaert N.V. Process and apparatus for desilvering a silver-containing solution
US5759377A (en) * 1995-07-15 1998-06-02 Agfa-Gevaert Process for de-silvering of a silver-containing solution
DE69524074T2 (de) * 1995-07-15 2002-07-04 Agfa Gevaert Nv Verfahren und Vorrichtung zur Entsilberung von Lösungen
GB9726534D0 (en) * 1997-12-17 1998-02-11 Eastman Kodak Co Determination of silver in a photographic solution

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1866701A (en) * 1929-03-13 1932-07-12 Eastman Kodak Co Method and apparatus for recovering silver from fixing solutions
DE1187806B (de) * 1962-03-21 1965-02-25 Bayer Ag Verfahren und Vorrichtung zur Silberrueckgewinnung aus Fixierbaedern
US4186067A (en) * 1974-06-26 1980-01-29 Ciba-Geigy Aktiengesellschaft Electrolytic recovery of silver from photographic bleach-fix baths
JPS5321048A (en) * 1976-08-10 1978-02-27 Nippon Electric Co Constant current density plating device
US4287044A (en) * 1980-03-31 1981-09-01 Silver Systems, Ltd. Silver recovery apparatus

Also Published As

Publication number Publication date
LU82188A1 (fr) 1981-09-10
US4377456A (en) 1983-03-22
DE3168559D1 (en) 1985-03-14
EP0035008A3 (en) 1982-06-09
ATE11602T1 (de) 1985-02-15
EP0035008A2 (de) 1981-09-02
JPS56138737A (en) 1981-10-29

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