EP0222252A2 - Procédé et dispositif pour préparer des émulsions photographiques à l'halogénure d'argent - Google Patents

Procédé et dispositif pour préparer des émulsions photographiques à l'halogénure d'argent Download PDF

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Publication number
EP0222252A2
EP0222252A2 EP86114942A EP86114942A EP0222252A2 EP 0222252 A2 EP0222252 A2 EP 0222252A2 EP 86114942 A EP86114942 A EP 86114942A EP 86114942 A EP86114942 A EP 86114942A EP 0222252 A2 EP0222252 A2 EP 0222252A2
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EP
European Patent Office
Prior art keywords
silver halide
collecting container
cleaning device
soluble
emulsion
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Withdrawn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
EP86114942A
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German (de)
English (en)
Other versions
EP0222252A3 (fr
Inventor
Klaus Dr. Hoffmann
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
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Agfa Gevaert AG
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Filing date
Publication date
Application filed by Agfa Gevaert AG filed Critical Agfa Gevaert AG
Publication of EP0222252A2 publication Critical patent/EP0222252A2/fr
Publication of EP0222252A3 publication Critical patent/EP0222252A3/fr
Withdrawn legal-status Critical Current

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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F23/00Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
    • B01F23/40Mixing liquids with liquids; Emulsifying
    • B01F23/49Mixing systems, i.e. flow charts or diagrams
    • GPHYSICS
    • G03PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03CPHOTOSENSITIVE MATERIALS FOR PHOTOGRAPHIC PURPOSES; PHOTOGRAPHIC PROCESSES, e.g. CINE, X-RAY, COLOUR, STEREO-PHOTOGRAPHIC PROCESSES; AUXILIARY PROCESSES IN PHOTOGRAPHY
    • G03C1/00Photosensitive materials
    • G03C1/005Silver halide emulsions; Preparation thereof; Physical treatment thereof; Incorporation of additives therein
    • G03C1/015Apparatus or processes for the preparation of emulsions
    • GPHYSICS
    • G03PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03CPHOTOSENSITIVE MATERIALS FOR PHOTOGRAPHIC PURPOSES; PHOTOGRAPHIC PROCESSES, e.g. CINE, X-RAY, COLOUR, STEREO-PHOTOGRAPHIC PROCESSES; AUXILIARY PROCESSES IN PHOTOGRAPHY
    • G03C1/00Photosensitive materials
    • G03C1/005Silver halide emulsions; Preparation thereof; Physical treatment thereof; Incorporation of additives therein
    • G03C1/015Apparatus or processes for the preparation of emulsions
    • G03C2001/0157Ultrafiltration

Definitions

  • the invention relates to a method and an apparatus for producing photographic silver halide emulsions.
  • silver halide emulsions To form light-sensitive silver halide emulsions, it is already known to precipitate corresponding silver salts in a binder.
  • the silver halide can be precipitated by adding an aqueous solution of a silver salt to a halide solution in gelatin.
  • the size of the silver halide grains obtained is controlled, inter alia, by the temperature of the solution, the run-in time and the excess of halide.
  • the advantages of ultrafiltration can only be fully exploited if the device can be used in fluid communication with the precipitation chamber and with the collection container.
  • the emulsion can be cleaned and concentrated economically before further processing (such as ripening, solidification or presentation as a seed crystal or as a partner for a redissolution) without uneconomical breaks for the transport and / or intermediate storage of the emulsion arise.
  • volume flow is understood here to mean the volume of liquid per unit time flowing through each cross section of a pipeline, measured, for example, in 1 / min.
  • the mass flow is accordingly the mass per unit of time, for example measured in kg / min.
  • the dwell time is understood to mean the volume of the precipitation space divided by the volume flow through this space.
  • Permeate output is understood to mean the volume flow of permeate, based on the unit of the filter surface, measured e.g. in 1 / (m2min).
  • nucleation phase it may be necessary to return the precipitate formed to the precipitation space over a short distance in order to allow it to grow to a stable particle size before being mixed with the total amount of the peptizer solution or emulsion in the collecting container .
  • a particularly preferred dispersant is water or a solution consisting essentially of water.
  • the photosensitive silver halide emulsion is prepared by reacting a soluble silver salt, in particular silver nitrate, with at least one soluble halide, in particular a water-soluble halide in aqueous solution.
  • the mass or volume flow of the silver halide emulsion circulating in the circulation system KS-1 is preferably greater, preferably at least by a factor of 1.2, than when entering the collecting container 3.
  • the reaction between the silver salts and halides is carried out in a precipitation chamber separate from the collecting container.
  • the silver halide emulsion from the collecting container 3 is at least partially returned to the circulation system KS-1.
  • the emulsion precipitated in the precipitation room 1 is temporarily led into the collecting container 3 while circumventing the circulation system KS-1.
  • the cleaning device can be temporarily emptied and rinsed.
  • the silver halide emulsion after passing through the cleaning device 2, is partly returned before and partly behind the precipitation chamber 1.
  • the feed into the collecting container 3 can be interrupted at least temporarily.
  • Suitable cleaning devices are those with which, in a continuous process, dispersants and molecules dissolved in them can be removed from the emulsion.
  • the cleaning device is an ultrafiltration device.
  • the ultrafiltration device preferably contains membranes made of inert, nonionic Polymers. These are suitable for removing soluble salts from photographic emulsions and, if appropriate, also concentrating these emulsions by reducing the volume by removing dispersant.
  • Suitable membranes can e.g. from polyvinyl acetate, polyvinyl alcohol, polyvinyl formate or polyvinyl ethers, such as e.g. Polyvinyl methyl or ethyl ethers, also from polyamides, polyimides, polyvinyl and polyvinylidene chloride, aromatic polymers, such as aromatic polyesters, or polytetrafluoroethylene.
  • membranes made of polyamides, polyvinyl chloride and polytetrafluoroethylene are preferred.
  • Membranes made from regenerated cellulose or cellulose esters, such as cellulose acetate or mixed cellulose esters, can also preferably be used for the process according to the invention.
  • the membranes preferably have a permeability for molecules with relative molecular weights of up to about 300,000, in particular up to about 50,000.
  • the gelatin-silver halide emulsions to be cleaned by the process according to the invention can be broad in terms of concentration of silver halide, gelatin content, salt content and pH Limits vary. In general, the content of soluble salts is 0.1 to 3 moles per liter of emulsion, depending on the production conditions.
  • the silver halide content can be 0.1 to 3 mol, preferably 0.1 to 1 mol, per 1 emulsion.
  • the gelatin concentration can be increased from 0.01% to 12%, preferably up to 8%, temperatures between 20 ° C. and 75 ° C., preferably 30 to 50 ° C. being maintained.
  • the pressure difference across the membrane is preferably between 0.3 and 4 bar.
  • the cleaning device 2 is an ultrafiltration device.
  • the device comprises an inlet 7 for the supply of water-soluble silver salts and a supply 8 for the supply of water-soluble halides into the reaction space 1. From this the emulsion with the precipitated silver halide is pump 5 after passing through the tap 18 into the circulation system KS-1 promoted, which has an additional pump 6 with which the throughput speed can be increased. After passing through the prefilter 4, the silver halide emulsion enters the cleaning device 2 (preferably an ultrafiltration device) and is partly led via the inlet 10 into the collecting container at the tap 17 and partly returned to the circulation system KS-1.
  • the circulation system KS-1 in this case comprises the three-way cocks 17 and 18, the pump 6, the prefilter 4 and the cleaning device 2.
  • a stirring device 9 is provided in the collecting container 3, from the collecting container the emulsion can be returned to the reaction chamber 1.
  • a device according to FIG. 1 can, however, also be used to produce silver halide emulsions by combining differently soluble silver halide emulsions.
  • the differently soluble silver halide emulsions can be added to the reaction space through the feeds 7 and 8. It is also possible to put at least one of these silver halide emulsions in reaction chamber 1.
  • the device shown in Figure 2 includes the following features:
  • a reaction partner or the dispersing medium can also be introduced into the collecting container 3 from a storage vessel 14 by means of the inlet 11. Furthermore, it is possible to guide the contents of the storage vessel 14 into the device via the multi-way valve 13.
  • the cleaning device 2 is in a separate circuit KS-1 which has the multi-way valve 13, the pump 6, the multi-way valve 12, the prefilter 4, the cleaning device 2 and the valve 17.
  • the multi-way valve 12 can be set so that first the pre-filter 4 and then the cleaning device 2 or first the cleaning device 2 and then the pre-filter 4 are passed through.
  • the silver halide precipitated in the precipitation chamber 1 can be fed into the circulation system KS-1 by means of the multi-way cock 13, but it is also possible to add the precipitated silver halide directly to the collecting container 3 bypassing the circulation system KS1, the shut-off device 21 is closed; with such a regulation, it is possible to clean the cleaning device 2 without interrupting the precipitation via the valves 19 and 20.
  • the device shown in FIG. 3 largely corresponds to the device from FIG. 1, it additionally contains the throttle valves 15, 16, 23 and 24 and offers the possibility of using the connecting piece 22 to create a circuit enclosing the filling space 1 with the exclusion of the collecting container 3.
  • a cleaning device in particular an ultrafiltration device
  • KS-1 a separate circulation system KS-1 it is possible to remove water-soluble compounds, in particular water-soluble salts, during the precipitation, during breaks in the precipitation and after the precipitation, and to concentrate the silver halide emulsion by removing water.
  • the precipitation is carried out in the presence of a protective colloid or binder.
  • a protective colloid or binder for example proteins, in particular gelatin, alginic acid or their derivatives such as esters, amides or salts, cellulose derivatives such as carboxymethyl cellulose and cellulose sulfates, starch or their derivatives or hydrophilic synthetic binders such as polyvinyl alcohol, partially saponified polyvinyl acetate and polyvinyl pyrrolidone.
  • the binders can also contain other synthetic binders in dissolved or dispersed form, such as homopolymers or copolymers of acrylic or methacrylic acid or their derivatives such as esters, amides or nitriles, and also vinyl polymers such as vinyl esters or vinyl ethers.
  • other synthetic binders in dissolved or dispersed form, such as homopolymers or copolymers of acrylic or methacrylic acid or their derivatives such as esters, amides or nitriles, and also vinyl polymers such as vinyl esters or vinyl ethers.
  • a gelatin / silver ratio of 0.01 to 1 is preferably maintained at the end of the precipitation.
  • Chloride, bromide and iodide or mixtures thereof can be used as the halide in the light-sensitive silver halide emulsions.
  • the crystals are predominantly compact, e.g. are cubic or octahedral or have transitional forms. They can be characterized in that they have a thickness of more than 0.2 ⁇ m at the end of the precipitation.
  • the average ratio of diameter to thickness is preferably less than 8: 1, it being true that the diameter of a grain is defined as the diameter of a circle with a circle content corresponding to the projected area of the grain.
  • all or individual emulsions can also have essentially tabular silver halide crystals in which the ratio of diameter to thickness is greater than 8: 1.
  • the emulsions can be chemically sensitized.
  • the usual sensitizers are suitable for chemical sensitization of the silver halide grains.
  • Sulfur-containing compounds for example allyl isothiocyanate, allyl thiourea and thiosulfates, are particularly preferred.
  • Precious metals or noble metal compounds such as gold, platinum, palladium, iridium, ruthenium or rhodium are also suitable as chemical sensitizers.
  • This method of chemical sensitization is in the article by R. Koslowsky. Z.Wiss.Phot. 46 , 65-72 (1951). It is also possible to use the Emul sensitize with polyalkylene oxide derivatives. Reference is also made to Research Disclosure No. 17 643, Section III.
  • the emulsions can be optically sensitized in a manner known per se, e.g. with the usual polymethine dyes, such as neutrocyanines, basic or acidic carbocyanines, rhodacyanines, hemicyanines, styryl dyes, oxonols and the like.
  • polymethine dyes such as neutrocyanines, basic or acidic carbocyanines, rhodacyanines, hemicyanines, styryl dyes, oxonols and the like.
  • Such sensitizers are from F.M. Hamer in "The Cyanine Dyes and related Compounds", (1964). In this regard, reference is made in particular to Ullmann's Encyclopedia of Technical Chemistry, 4th Edition, Volume 18, pages 431 ff and to Research Disclosure No. 17 643, Section IV.
  • antifoggants and stabilizers can be used.
  • Particularly suitable stabilizers are azaindenes, preferably tetra- or penta-azaindenes, especially those which are substituted with hydroxyl or amino groups.
  • Such connections are, for example, in the article by Birr, Z.Wiss.Phot. 47 , 1952), pp. 2-58.
  • Other suitable stabilizers and antifoggants are given in Research Disclosure No. 17,643 in Section IV.
  • the emulsions can be hardened in the usual manner, for example with hardeners of the epoxy type, the heterocyclic ethylene imine and the acryloyl type. Furthermore, it is also possible to harden according to the process of German Offenlegungsschrift 2 218 009 to color photographic To achieve materials that are suitable for high temperature processing. It is also possible to harden with hardeners of the diazine, triazine or 1,2-dihydroquinoline series or with hardeners of the vinyl sulfone type. Further suitable hardening agents are known from German laid-open documents 2 439 551, 2 225 230, 2 317 672 and from Research Disclosure 17 643, section XI.
  • silver halide emulsions of virtually any type can be precipitated according to the invention.
  • both homodisperse and heterodisperse silver halide emulsions can be prepared by the process according to the invention.
  • Homodisperse emulsions are understood to mean those with a narrow particle size distribution; preferably at least 95% of the silver halide grains have a diameter which does not deviate from the mean grain diameter by more than 40%, or preferably not more than 30%.
  • the silver halide grains can have any of the known forms, for example cubic, octahedral or else a tetradecahedral mixed form.
  • Heterodisperse emulsions are to be understood in particular to be those in which at least 10%, but preferably at least 20%, of the silver halide grains have a diameter which deviates from the mean grain diameter by at least 40%.
  • the absolute value of the average grain size of the metal salts produced according to the invention, in particular of the silver halide emulsions produced according to the invention, can vary within wide limits.
  • both fine-grain silver halide emulsions with an average diameter of less than 0.5 ⁇ m, preferably less than 0.3 ⁇ m, and coarse-grain ones with average grain diameters between 0.5 and 4 ⁇ m can be produced.
  • emulsions can in principle be produced for a wide variety of photographic materials, such as, for example, negative-working emulsions with high surface sensitivity, negative-working emulsions with high internal sensitivity, direct-positive-working emulsions that can be superficially veiled or superficially unveiled, print-out emulsions, reverse emulsions, emulsions for black / white and for color materials, emulsions with defined grain size distribution and halide topography, especially with defined halide, especially iodide gradients.
  • photographic materials such as, for example, negative-working emulsions with high surface sensitivity, negative-working emulsions with high internal sensitivity, direct-positive-working emulsions that can be superficially veiled or superficially unveiled, print-out emulsions, reverse emulsions, emulsions for black / white and for color materials, emulsions with defined grain size distribution and halide topography, especially with defined hal
  • a monodisperse AgBr emulsion of predominantly cubic crystal garb is produced using the device shown in FIG. 1 in two steps (seed crystal precipitation and precipitation) as follows:
  • Cleaning device 2 is an ultrafiltration module with membranes made of polysulfone with a separation limit of 50,000 and a filter area of 1.4 m2.
  • a stainless steel screen serves as the prefilter 4.
  • 5 and 6 are centrifugal pumps.
  • the pump 5 has a delivery rate of 40 l / min
  • pump 6 has a delivery rate of 100 l / min.
  • a solution (1) consisting of 9 l of water and 260 g of an inert bone gelatin.
  • the following serve as partners for the precipitation crystallization: a solution (2) of 3670 g of silver nitrate and 6 l of water and a solution (3) of 2570 g of potassium bromide and 6.1 l of water.
  • Solutions (2) and (3) are metered into the reaction space 1 via the lines 7 and 8, initially with a volume flow of 120 ml / min. After 5 minutes, the inlet volume flow is reduced to approx. 60 ml / min. With the help of the pump 5, while the inlets 7 and 8 are open, a volume flow of approx. 40 l / min is maintained by the circuit 3/1/5/18/17/10. The unused parts of the separate circuit are filled with water during this time.
  • the pAg value in the collecting container is kept at the value 6.9 during the precipitation by fine control of the inlet 8.
  • the temperature in the collection container is kept at 50 ° C.
  • the inlets 7 and 8 are closed and the separate circuit is put into operation in that the pump 6 is switched on and the shut-off elements 17 and 18 are switched over in such a way that the emulsion has the optimum volume flow rate for ultrafiltration 90 l / min flows through the cleaning device 2, with a constant low flow (40 l / min) through the collecting container 3.
  • a permeate flow of initially 1 l / min is achieved in this way.
  • the emulsion is concentrated by withdrawing 15 l of permeate and then diafiltered at constant volume by replacing the draining permeate with demineralized water. 20 l of this water are required for desalination.
  • this cleaning phase there are only approx. 3 l in the collection container. Nevertheless, there is no foam in the open container.
  • the circuits are emptied and the emulsion is brought together in the collection container.
  • the temperature in the collecting container is kept at 60 ° C, the pAg value at 6.7.
  • the subsequent cleaning and concentration is carried out in the same way as for seed crystal precipitation.
  • An emulsion with an average grain size of 0.48 ⁇ m, an AgBr concentration of 393 g / kg and a gelatin / AgBr mass ratio of 0.04 is obtained.
  • a mixture (6) consisting of 4 l of water, 218 g of an inert gelatin and 1.88 kg of the emulsion according to Example 1.2 as seed crystal precipitation.
  • the following precipitation partners are used: a solution (7) made from 5000 g silver nitrate and 8.1 l water and a solution (8) made from 3500 g potassium bromide and 8.2 l water.
  • the inlet volume flow is now 50 ml / min, the emulsion flow through the reaction space as in Example 1.
  • the temperature in the collecting container is kept at 70 ° C., the pAg value at 6.5.
  • the separate circuit KS-1 is switched on, which was previously filled with water. While a volume flow of 100 l / min is generated in this cleaning circuit, the volume flow through the collecting container 3 is kept constant at 40 l / min until the end of the inlets 7 and 8 after a total of 160 min infeed time. The transport of the emulsion through the reaction space 1 simultaneously leads to its feeding into the cleaning device 2.
  • Switching on the ultrafiltration device removes 100 ml of permeate per minute from the emulsion, i.e. the volume flow of the permeate is restricted to this value by a throttle valve (not shown).
  • the emulsion is cleaned at a permeate flow of 600 ml / min with simultaneous addition of deionized water at a constant volume with a throughput of 25 l.
  • Emulsion with an average grain size of 1 ⁇ m and a silver bromide concentration of 346 g per kg is obtained Emulsion and a gelatin / silver bromide mass ratio of 0.04.
  • the emulsion thus produced in one operation no longer requires additional desalination for further processing.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)
  • Silver Salt Photography Or Processing Solution Therefor (AREA)
EP86114942A 1985-11-09 1986-10-28 Procédé et dispositif pour préparer des émulsions photographiques à l'halogénure d'argent Withdrawn EP0222252A3 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE19853539845 DE3539845A1 (de) 1985-11-09 1985-11-09 Verfahren und vorrichtung zur herstellung fotografischer silberhalogenidemulsionen
DE3539845 1985-11-09

Publications (2)

Publication Number Publication Date
EP0222252A2 true EP0222252A2 (fr) 1987-05-20
EP0222252A3 EP0222252A3 (fr) 1988-06-22

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EP86114942A Withdrawn EP0222252A3 (fr) 1985-11-09 1986-10-28 Procédé et dispositif pour préparer des émulsions photographiques à l'halogénure d'argent

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Country Link
US (1) US4758505A (fr)
EP (1) EP0222252A3 (fr)
JP (1) JPS62113137A (fr)
DE (1) DE3539845A1 (fr)

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0423538A1 (fr) * 1989-10-16 1991-04-24 Minnesota Mining And Manufacturing Company Procédé pour la préparation des émulsions photosensibles à l'halogénure d'argent
EP0577886A1 (fr) * 1992-07-10 1994-01-12 Agfa-Gevaert N.V. Préparation des émulsions à grains tabulaires avec un indice de form intermédiaire
EP0585180A1 (fr) * 1992-07-24 1994-03-02 Eastman Kodak Company Procédé d'ultrafiltration à temps de cycle fixe
EP0589323A1 (fr) * 1992-09-24 1994-03-30 Agfa-Gevaert Ag Matériau photographique couleur à l'halogénure d'argent
EP0779538A1 (fr) * 1995-12-14 1997-06-18 Kodak-Pathe Procédé pour préparer une émulsion photographique et appareil pour la mise en oeuvre du procédé
EP0779537A1 (fr) * 1995-12-14 1997-06-18 Kodak-Pathe Procédé pour préparer une émulsion photographique et appareil pour la mise en oeuvre du procédé

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Publication number Priority date Publication date Assignee Title
US5164092A (en) * 1991-02-20 1992-11-17 Eastman Kodak Company 2-stage ultrafiltration process for photographic emulsions
US5248418A (en) * 1991-02-20 1993-09-28 Eastman Kodak Company 2-stage ultrafiltration system for photographic emulsions
US5411715A (en) * 1992-06-09 1995-05-02 Eastman Kodak Company Apparatus for preparing aqueous amorphous particle dispersions of high-melting microcrystalline solids
US5334496A (en) * 1992-09-17 1994-08-02 Eastman Kodak Company Process and apparatus for reproducible production of non-uniform product distributions
JPH07319094A (ja) * 1994-03-31 1995-12-08 Konica Corp 脱塩方法、脱塩濃縮方法及び微粒子供給方法ならびにハロゲン化銀写真乳剤及びハロゲン化銀写真感光材料
FR2737022B1 (fr) * 1995-07-20 2003-02-07 Kodak Pathe Procede et dispositif de traitement d'un film photographique
US5928853A (en) * 1996-08-29 1999-07-27 Konica Corporation Method of manufacturing silver halide emulsion
FR2812218B1 (fr) * 2000-07-28 2003-01-10 Eastman Kodak Co Procede pour ameliorer le fonctionnement d'une membrane d'un dispositif de nanofiltration

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FR687074A (fr) * 1929-12-21 1930-08-04 Procédé de fabrication d'une émulsion gélatineuse ultramicroscopique photographique
DE2444159B1 (de) * 1974-09-16 1975-09-18 Fa. Otto Duerr, 7000 Stuttgart Verfahren und Anlage zur Aufbereitung von Emulsionen, insbesondere Öl-Emulsionen
US4334012A (en) * 1980-01-30 1982-06-08 Eastman Kodak Company Silver halide precipitation process with deletion of materials

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US3206313A (en) * 1961-05-15 1965-09-14 Eastman Kodak Co Chemically sensitized emulsions having low surface sensitivity and high internal sensitivity
GB1356921A (en) * 1970-04-03 1974-06-19 Agfa Gevaert Preparation of silver halide emulsions
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DE2340082C3 (de) * 1972-08-14 1980-03-06 E.I. Du Pont De Nemours And Co., Wilmington, Del. (V.St.A.) Verfahren zur Herstellung einer fotografischen Silberhalogenidemulsion
GB1591608A (en) * 1976-09-14 1981-06-24 Agfa Gevaert Method and apparatus suitable for the preparation of silver halide emulsions
US4336328A (en) * 1981-06-11 1982-06-22 Eastman Kodak Company Silver halide precipitation process with deletion of materials through the reaction vessel
US4539290A (en) * 1983-09-27 1985-09-03 E. I. Du Pont De Nemours And Company Process for pulsed flow, balanced double jet precipitation
JPS60122935A (ja) * 1983-12-07 1985-07-01 Konishiroku Photo Ind Co Ltd ハロゲン化銀乳剤の製造方法
EP0144990B1 (fr) * 1983-12-08 1990-04-25 Fuji Photo Film Co., Ltd. Procédé pour la fabrication d'émulsion aux halogénures d'argent

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FR687074A (fr) * 1929-12-21 1930-08-04 Procédé de fabrication d'une émulsion gélatineuse ultramicroscopique photographique
DE2444159B1 (de) * 1974-09-16 1975-09-18 Fa. Otto Duerr, 7000 Stuttgart Verfahren und Anlage zur Aufbereitung von Emulsionen, insbesondere Öl-Emulsionen
US4334012A (en) * 1980-01-30 1982-06-08 Eastman Kodak Company Silver halide precipitation process with deletion of materials

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Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0423538A1 (fr) * 1989-10-16 1991-04-24 Minnesota Mining And Manufacturing Company Procédé pour la préparation des émulsions photosensibles à l'halogénure d'argent
EP0577886A1 (fr) * 1992-07-10 1994-01-12 Agfa-Gevaert N.V. Préparation des émulsions à grains tabulaires avec un indice de form intermédiaire
EP0585180A1 (fr) * 1992-07-24 1994-03-02 Eastman Kodak Company Procédé d'ultrafiltration à temps de cycle fixe
EP0589323A1 (fr) * 1992-09-24 1994-03-30 Agfa-Gevaert Ag Matériau photographique couleur à l'halogénure d'argent
EP0779538A1 (fr) * 1995-12-14 1997-06-18 Kodak-Pathe Procédé pour préparer une émulsion photographique et appareil pour la mise en oeuvre du procédé
EP0779537A1 (fr) * 1995-12-14 1997-06-18 Kodak-Pathe Procédé pour préparer une émulsion photographique et appareil pour la mise en oeuvre du procédé
FR2742558A1 (fr) * 1995-12-14 1997-06-20 Kodak Pathe Procede pour preparer une emulsion photographique et appareil pour la mise en oeuvre du procede
FR2742557A1 (fr) * 1995-12-14 1997-06-20 Kodak Pathe Procede pour preparer une emulsion photographique et appareil pour la mise en oeuvre du procede
US5709990A (en) * 1995-12-14 1998-01-20 Eastman Kodak Company Method for preparing a photographic emulsion, and apparatus for implementing the method
US5723279A (en) * 1995-12-14 1998-03-03 Eastman Kodak Company Method for preparing a photographic emulsion, and apparatus for implementing the method

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US4758505A (en) 1988-07-19
DE3539845A1 (de) 1987-05-14
EP0222252A3 (fr) 1988-06-22
JPS62113137A (ja) 1987-05-25

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