EP0301579B1 - Methode und Apparat zur Verarbeitung von photographischen photoempfindlichen Lösungen - Google Patents

Methode und Apparat zur Verarbeitung von photographischen photoempfindlichen Lösungen Download PDF

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Publication number
EP0301579B1
EP0301579B1 EP88112348A EP88112348A EP0301579B1 EP 0301579 B1 EP0301579 B1 EP 0301579B1 EP 88112348 A EP88112348 A EP 88112348A EP 88112348 A EP88112348 A EP 88112348A EP 0301579 B1 EP0301579 B1 EP 0301579B1
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EP
European Patent Office
Prior art keywords
valve
flow control
control valves
flow
photographic photosensitive
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
EP88112348A
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English (en)
French (fr)
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EP0301579A2 (de
EP0301579A3 (en
Inventor
Yasunori Fuji Photo Film Co. Ltd. Ichikawa
Hiroshi Fuji Photo Film Co. Ltd. Ohnishi
Akira Fuji Photo Film Co. Ltd. Kojima
Akira Fuji Photo Film Co. Ltd. Kato
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.)
Fujifilm Holdings Corp
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Fuji Photo Film Co Ltd
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Filing date
Publication date
Application filed by Fuji Photo Film Co Ltd filed Critical Fuji Photo Film Co Ltd
Publication of EP0301579A2 publication Critical patent/EP0301579A2/de
Publication of EP0301579A3 publication Critical patent/EP0301579A3/en
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Publication of EP0301579B1 publication Critical patent/EP0301579B1/de
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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
    • G03C1/00—Photosensitive materials
    • G03C1/005—Silver halide emulsions; Preparation thereof; Physical treatment thereof; Incorporation of additives therein
    • G03C1/015—Apparatus or processes for the preparation of emulsions
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
    • B01F35/20—Measuring; Control or regulation
    • B01F35/21—Measuring
    • B01F35/211—Measuring of the operational parameters
    • B01F35/2111—Flow rate
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
    • B01F35/20—Measuring; Control or regulation
    • B01F35/21—Measuring
    • B01F35/2132—Concentration, pH, pOH, p(ION) or oxygen-demand
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
    • B01F35/80—Forming a predetermined ratio of the substances to be mixed
    • B01F35/82—Forming a predetermined ratio of the substances to be mixed by adding a material to be mixed to a mixture in response to a detected feature, e.g. density, radioactivity, consumed power or colour
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
    • B01F23/40—Mixing liquids with liquids; Emulsifying

Definitions

  • the present invention relates to photographic photosensitive solution manufacturing method and apparatus for practicing such a method, in accordance with independent claims 1 and 6. More particularly, the invention relates to a method for mixing Ag+ and X ⁇ solutions to produce crystals of silver halide emulsion in a photographic photosensitive solution manufacturing process, and to an apparatus for practicing such a method.
  • Examples of a conventional method for adding Ag+ and X ⁇ solutions to produces crystals of silver halide emulsion in a photographic photosensitive solution manufacturing process and a conventional apparatus for practicing such a method include a method and apparatus in which the addition is controlled by means of a pump (see, for instance, U.S. Pats. No. 4,147,551 and 4,251,627) and a method and apparatus in which the addition is controlled by means of a control valve (see, for instance, U.S. Pats. Nos. 3,692,283, 3,897,935, 3,999,048, 4,026,668 and 4,031,912).
  • Document US-A-3,821,002 discloses a method for establishing and maintaining an equilibrium flow rate of a silver or a halide salt solution prior to delivery thereof into a precipitation vessel containing a peptizer solution to provide a preselected pAg value during the preparation of a silver halide emulsion, whereby utilizing flow meters for monitoring the flow rate of the salt solution and means for detecting the pAg in the precipitation vessel and a three-way diaphragm control valve.
  • an object of the invention is to eliminate the above-described difficulties. More specifically, an object of the invention is to provide a photographic photosensitive solution manufacturing method and apparatus in which Ag+ and X ⁇ solutions are added together and by which a variety of different photosensitive solutions can be manufactured, the equipment can be easily operated, and flow control valves employed in the apparatus are capable of controlling the addition of Ag+ and X ⁇ in such a manner as to manufacture silver halide emulsion crystals uniform both in size and shape.
  • Fig. 1 illustrates schematically a photographic photosensitive solution manufacturing method and apparatus according to the present invention.
  • the apparatus includes a raw material storage tank 10 containing Ag+ solution prepared in advance, a raw material storage tank 11 containing an X ⁇ solution also prepared in advance, flow control valves 12a and 12b, flow meters 13a and 13b, stop valves 14a and 14b connected to pipes extending from the respective raw material storage tanks 10 and 11, a precipitation vessel 16 which receives the Ag+ and X ⁇ solutions from the raw material storage tanks 10 and 11 and agitates them for reaction, and a controller 15 which receives feedback signals from the flow meters 13a and 13b and from a pAg potentiometer 17 mounted in the precipitation vessel 16 and in response controls the flow control valves 12a and 12b in accordance with a predetermined program.
  • each of the flow control valves 12a and 12b is constructed as shown in Figs. 2 and 3. More specifically, each of the flow control valves 12a and 12b includes a cylindrically or conically elongated valve head 21 in a valve casing 22, the valve head 21 having a stroke H which completely disengages the valve head 21 from its valve seat 23. The valve head 21 is moved by a servo motor 24.
  • Rotational motion of the motor 24 is transmitted through a feed screw mechanism to a coupling plate 25 so as to move the latter up and down.
  • the coupling plate 25 is connected to the valve shaft 26. Therefore, the valve shaft 26 is moved up and down as the coupling plate is moved up and down.
  • the cylindrically or conically shaped valve head 21 formed on a circular truncated cone which tapers towards the outlet of the valve is positioned on the outlet side of the valve casing.
  • the rate of change of the flow rate with the valve stroke measured between the valve head 21 and the valve seat 23 is small and linear.
  • the opening stroke of the valve takes place in the long inlet side of the valve casing, thus allowing the valve seat 23 to be made large.
  • the valve head 21 is moved by the servo motor 24, as has been previously described.
  • the valve head 21 is lifted by the servo motor 24 (having the valve characteristic curve c in Fig. 4).
  • the flow valve used in the practice of the invention has a flow control range about fifty times as large and has a smaller and more linear rate of change of flow rate with valve stroke compared with conventional valves, the characteristics of which is indicated by a and b in Fig. 4.
  • the prepared Ag+ and X ⁇ solutions are held at the respective stop valves 14a and 14b before the start of addition, while the flow control valves 12a and 12b are automatically set at positions corresponding to the flow rates at the start of addition as determined by the particular type of solution to be prepared.
  • the flow control valves 12a and 12b can be accurately automatically set because their rate of change of flow rate with the degree of valve opening is smaller than in the case of other flow valves.
  • the stop valves 14a and 14b are opened, thus starting the addition operation.
  • the flow meters 13a and 13b feed back measured values to the controller 15.
  • the controller 15 compares the fed-back values with the set values, and controls the flow control valves 12a and 12b so that the fed-back values are made equal to the set values.
  • the controller 15 may receive the pAg potential output signal from the pAg potentiometer 17 and control the flow control valves 12a and 12b in such a manner that the pAg potential output signal is held equal to the set value.
  • the flow control range from the fully closed position of the valves to the fully opened position is wide since the valve structure produces a very low resistance to the fluid flow, and because the valve stroke is long, the configuration of the valve head allows the flow rate to change linearly with the valve stroke. Therefore, even an extremely small flow change can be precisely controlled. Furthermore, since a servo motor is employed for lifting the valve head, valve control can be achieved easily and quickly. Therefore, the flow control program can be implemented precisely and quickly, and for production of a variety of photographic photosensitive solutions, the silver halide emulsion crystals can be made to have a uniform size and shape.
  • solutions I and II were prepared on a scale of 1.2 times the prescribed amounts.
  • the adding condition was such that solution II was added at a constant flow rate of 2 liters/min and solution III was controlled so that P Ag in the vessel was maintained at 8.8
  • the addition process was ended at the time when the total addition time for solution II became equal to that in the method and apparatus of the invention.
  • a single-loop controller manufactured by Toshiba Co. was employed to determine the PID value with which the best control conditions could be obtained.
  • the control conditions thus obtained were applied to all solutions.
  • the pump used in the tests was a gear pump manufactured by Marg Co. The same agitating conditions were applied to all solutions.
  • Example I The same solutions as in Example I were used to compare diaphragm type control valves with the flow control valves of the invention.
  • the aforementioned single-loop controller manufactured by Toshiba Co. was employed.
  • Diaphragm type control valves manufactured by Yamatake Honeywell were used for comparisons.
  • the pAg potential variation range can be made small, as a result of which the silver halide emulsion particles are sharp in size distribution and uniform in shape.
  • the flow control valves are simple both in configuration and in construction, and can be applied to the production of a variety of photographic photosensitive solutions. Furthermore, the flow control valves are advantageous in that the times required for switching them or cleaning them are greatly reduced, and their flow control range is wide. As a result, the addition of Ag+ and X ⁇ solutions can be achieved without significant residual loss.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physics & Mathematics (AREA)
  • Fluid Mechanics (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • General Physics & Mathematics (AREA)
  • Flow Control (AREA)
  • Accessories For Mixers (AREA)

Claims (10)

  1. Verfahren zur Herstellung einer photographischen photosensitiven Lösung, das folgende Schritte umfaßt:
    Herstellung von Ag⁺- und von X⁻-Lösung im voraus und Zuführen der Ag⁺- und der X⁻-Lösung in jeweilige Speichertanks (10,11);
    Bereitstellen von jeweiligen motorgesteuerten Durchflußreglern (12a,12b) für die Speichertanks und Steuern der Durchflußregler, um die Ag⁺- und die X⁻-Lösung aus den Speichertanks (10,11) einem Ausfällbehälter (16) in bestimmten Raten gemäß einem bestimmten Programm zuzuführen, wobei
    die Durchflußregler einen elektrischen Motor (24) umfassen;
    einen Vorschubspindelmechanismus und eine Koppelplatte (25), um die Motorrotation in eine Linearbewegung zu wandeln;
    einen Ventilschaft (26), der mit der Koppelplatte verbunden ist, um den Ventilschaft vertikal zu bewegen;
    und ein Ventilgehäuse (22) mit einem Ventilsitz (23), der darin ausgebildet ist, und das ein Einlaßseitengehäuse umfaßt, wobei der Ventilschaft (26) sich entlang einer Mittelachse des Einlaßseitengehäuses erstreckt, und ein Auslaßseitengehäuse, das mit dem Einlaßseitengehäuse zusammentrifft;
    einen Ventilkörper, der mit dem Ventilschaft (26) verbunden ist, wobei der Ventilkörper eine Arbeitsfläche in Form eines runden Kegelstumpfes umfaßt, der zu einem Auslaß des Ventils zuläuft, und einen Ventilkopf (21), der in dem Auslaßseitengehäuse angebracht ist, wobei der Ventilkopf zylindrisch oder konisch geformt ist, so daß die Änderungsrate der Durchflußrate in bezug auf den Ventilhub (H) eine lineare Funktion mit geringer Steigung ist, und ein Ventilhub (H) zur vollständigen Öffnung des Ventilsitzes in dem Einlaßseitengehäuse erfolgt.
  2. Verfahren zum Herstellen einer photographischen photoempfindlichen Lösung nach Anspruch 1, wobei das Programm ein Durchflußratenprogramm der Form Q = at² bt + c ist, wobei Q die Durchflußrate, t die Zeit, und a, b, und c Konstanten sind.
  3. Verfahren zur Herstellung einer photographischen photosensitiven Lösung nach Anspruch 2, das weiter folgende Schritte umfaßt: Bereitstellen von Durchflußmessern (13a,13b) zum Messen der Durchflußrate der Ag⁺- und der X⁻-Lösung von den Speichertanks (10,11) in den Ausfällbehälter (17), und wobei der Schritt des Steuerns der Durchflußregler eine Rückkopplungsregelung der Durchflußregler (12a,12b) gemäß Ausgangssignalen von den Durchflußmessern und dem bestimmten Programm umfaßt.
  4. Verfahren zum Herstellen von einer photographischen photosensitiven Lösung nach Anspruch 1, wobei das Programm ein pAg-Potential-Programm der Form E = ℓt² + mt + n ist, wobei E das pAg-Potential in dem Ausfällbehältnis ist, t die Zeit, und ℓ, m und n Konstanten sind.
  5. Verfahren zum Herstellen einer photographischen photosensitiven Lösung nach Anspruch 4, das weiter folgende Schritte umfaßt: Bereitstellen eines pAg-Potentiometers (17) zum Messen eines pAg-Potentials in dem Ausfällbehälter (16), und wobei der Schritt des Steuerns der Durchflußregler (12a,12b) eine Rückkoppelungsregelung der Durchflußregler gemäß den Ausgangssignalen des pAg-Potentiometers (17) und dem bestimmten Programm umfaßt.
  6. Vorrichtung zum Herstellen einer photographischen photosensitiven Lösung, die folgendes umfaßt:
    jeweilige Speichertanks für Ausgangsmaterial (10,11) zum Speichern von vorab hergestellter Ag⁺- und X⁻-Lösung;
    wobei der Auslaß eines jeden Tanks mit einem Durchflußregler (12a,12b) verbunden ist, um eine Auslaßdurchflußrate sowohl von der Ag⁺- als auch von der X⁻-Lösung aus den jeweiligen Tanks zu steuern;
    einen Ausfällbehälter (16) zum Zusammenführen der Ag⁺- und der X⁻-Lösung, die durch die Durchflußregler (12a,12b) erhalten werden;
    eine Einrichtung zum Bewegen der zusammengeführten Ag⁺- und X⁻-Lösung in dem Ausfällbehälter; und
    eine Steuerung (15) zum Steuern der Durchflußregler gemäß einem bestimmten Programm,
    wobei jeder der Durchflußregler (12a,12b) folgendes umfaßt;
    einen elektrischen Motor (24);
    einen Vorschubspindelmechanismus und eine Koppelplatte (25) zum Umwandeln der Motorrotation in eine lineare Bewegung;
    einen Ventilschaft (26) der mit der Koppelplatte (25) verbunden ist um den Ventilschaft vertikal zu bewegen;
    ein Ventilgehäuse (22), das einen Ventilsitz (23) aufweist, der darin ausgebildet ist, und ein Einlaßseitengehäuse umfaßt, wobei der Ventilschaft (26) sich entlang einer Mittelachse des Einlaßseitengehäuses erstreckt, und ein Auslaßseitengehäuse, das mit dem Einlaßseitengehäuse zusammentrifft;
    einen Ventilkörper, der mit dem Ventilschaft (26) verbunden ist, wobei der Ventilkörper eine Arbeitsfläche in Form eines runden Kegelstumpfes umfaßt, der zu einem Auslaß des Ventils zuläuft, und einen Ventilkopf (21), der in dem Auslaßseitengehäuse angebracht ist, wobei der Ventilkopf zylindrisch oder konisch ausgebildet ist, so daß die Änderungsrate der Durchflußrate in bezug auf den Ventilhub (H) eine lineare Funktion mit geringer Steigung ist, und ein Ventilhub (H) zum vollständigen Öffnen des Ventilsitzes in dem Einlaßseitengehäuse erfolgt.
  7. Vorrichtung zum Herstellen einer photographischen photosensitiven Lösung nach Anspruch 6, die weiter umfaßt: Durchflußmesser (13a,13b) zum Messen der Durchflußraten durch jeden der Durchflußregler (12a,12b), wobei die Steuerung (15) die Durchflußregler gemäß den Ausgangssignalen von den Durchflußmessern und dem bestimmten Programm steuert.
  8. Vorrichtung zum Herstellen einer photographischen photosensitiven Lösung nach Anspruch 6, die weiter ein pAg-Potentiometers (17) umfaßt, das in dem Ausfällbehälter (16) angebracht ist um ein pAg-Potential in dem Ausfällbehälter zu messen, wobei die Steuerung (15) jeden der Durchflußregler (12a,12b) gemäß einem Ausgangssignal des pAg-Potentiometers und dem bestimmten Programm steuert.
  9. Vorrichtung zum Herstellen einer photographischen photosensitiven Lösung nach Anspruch 6, wobei der Ventilkopf (21) zylindrisch geformt ist.
  10. Vorrichtung zum Herstellen einer photographischen photosensitiven Lösung nach Anspruch 6, wobei der Ventilkopf (21) konisch ausgebildet ist.
EP88112348A 1987-07-30 1988-07-29 Methode und Apparat zur Verarbeitung von photographischen photoempfindlichen Lösungen Expired - Lifetime EP0301579B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP188736/87 1987-07-30
JP62188736A JPS6433545A (en) 1987-07-30 1987-07-30 Method and apparatus for producing photographic sensitive solution

Publications (3)

Publication Number Publication Date
EP0301579A2 EP0301579A2 (de) 1989-02-01
EP0301579A3 EP0301579A3 (en) 1990-11-28
EP0301579B1 true EP0301579B1 (de) 1994-12-28

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EP88112348A Expired - Lifetime EP0301579B1 (de) 1987-07-30 1988-07-29 Methode und Apparat zur Verarbeitung von photographischen photoempfindlichen Lösungen

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EP (1) EP0301579B1 (de)
JP (1) JPS6433545A (de)
DE (1) DE3852586T2 (de)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2687180B2 (ja) * 1989-08-10 1997-12-08 富士写真フイルム株式会社 ハロゲン化銀乳剤の製造方法
US5248577A (en) * 1990-08-13 1993-09-28 Eastman Kodak Company Reactant concentration control method and apparatus for precipitation reactions

Family Cites Families (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
BE791323A (fr) * 1971-11-15 1973-03-01 American Air Filter Co Registre de commande du debit d'un gaz
US3821002A (en) * 1972-03-06 1974-06-28 Eastman Kodak Co Process control apparatus and method for silver halide emulsion making
US4026668A (en) * 1973-12-20 1977-05-31 Eastman Kodak Company Control apparatus for silver halide emulsion making
US3999048A (en) * 1974-09-09 1976-12-21 E. I. Du Pont De Nemours And Company Flow control system for the precipitation of silver halide emulsions
JPS58121381A (ja) * 1982-01-13 1983-07-19 Matsushita Electric Ind Co Ltd 流体制御弁
US4575047A (en) * 1984-01-24 1986-03-11 Kennecott Corporation Ceramic to metal junction and method of making same

Also Published As

Publication number Publication date
DE3852586T2 (de) 1995-05-04
EP0301579A2 (de) 1989-02-01
DE3852586D1 (de) 1995-02-09
EP0301579A3 (en) 1990-11-28
JPS6433545A (en) 1989-02-03

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