EP0472007A1 - Photographic chemicals with reduced dust fraction - Google Patents

Photographic chemicals with reduced dust fraction Download PDF

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Publication number
EP0472007A1
EP0472007A1 EP91112641A EP91112641A EP0472007A1 EP 0472007 A1 EP0472007 A1 EP 0472007A1 EP 91112641 A EP91112641 A EP 91112641A EP 91112641 A EP91112641 A EP 91112641A EP 0472007 A1 EP0472007 A1 EP 0472007A1
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Prior art keywords
photographic processing
compound
dust
formula
alkyl
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EP91112641A
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German (de)
French (fr)
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EP0472007B1 (en
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Karl-Heinz Reuter
Manfred Dr. Reichrath
Heinz Dr. Meckl
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Agfa Gevaert AG
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Agfa Gevaert AG
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    • G—PHYSICS
    • G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03C—PHOTOSENSITIVE MATERIALS FOR PHOTOGRAPHIC PURPOSES; PHOTOGRAPHIC PROCESSES, e.g. CINE, X-RAY, COLOUR, STEREO-PHOTOGRAPHIC PROCESSES; AUXILIARY PROCESSES IN PHOTOGRAPHY
    • G03C5/00—Photographic processes or agents therefor; Regeneration of such processing agents
    • G03C5/26—Processes using silver-salt-containing photosensitive materials or agents therefor
    • G03C5/264—Supplying of photographic processing chemicals; Preparation or packaging thereof
    • G03C5/265—Supplying of photographic processing chemicals; Preparation or packaging thereof of powders, granulates, tablets

Definitions

  • the invention relates to solid-formulated photographic chemicals with a reduced dust content and a process for their production.
  • Photographic processing baths e.g. Developmental, bleaching and fixing baths usually contain the required active ingredients in low concentrations and are therefore prepared by the user himself from water and chemical concentrates as well as, if necessary, other auxiliaries.
  • the concentrates should be dosed as simply as possible and should be largely dust-free. In addition, no unnecessarily high costs should arise for packaging and transport.
  • the liquid concentrates which are generally used in practice for the production of ready-to-use photographic baths have the advantage over the previously used, powdered products that no dust development and no solution problems occur.
  • the concentrates have the disadvantages of the high proportion by weight and volume of water, as well as difficulties in disposing of the bulky packaging.
  • the object of the invention is therefore to find means with which photographic processing chemicals formulated in solid form can be produced, the dust content of which is reduced, and which are therefore dust-free or at least low-dust.
  • the products manufactured in this way should also dissolve in water in a short time.
  • Formulations that are free of or low in solids with a grain size ⁇ 0.1 mm are referred to as dust-free or low-dust.
  • the amount is determined by conventional sieve analysis; it should preferably be below 2% by weight, in particular below 1% by weight.
  • Suitable compounds of formula 1 are ethylene glycol, homologues of ethylene glycol and polyethylene glycols with average molecular weights from 200 to 10,000 and propylene glycol and polypropylene glycols with average molecular weights from 200 to 10,000, preferably polyethylene glycols with average molecular weights from 300 to 1,000, e.g. Polyethylene glycol 300, 400, 600 and 1,000; Short designation P 300, P 400, P 600, P 1000.
  • Suitable compounds of the formula 11 are fatty alcohols such as 1-dodecanol or fatty alcohol mixtures, for example a mixture with equal proportions of C 2 and C 4 fatty alcohol.
  • Suitable photographic processing chemicals are black and white developers, color developers, bleaching agents, fixing agents, bleach-fixing agents and stabilizers.
  • these photographic processing chemicals contain the usual active substances and auxiliaries. Details can be found in the exemplary embodiments.
  • the process for the preparation of the dedusted products according to the invention is characterized in that active ingredients and auxiliaries of a photographic processing bath are mixed together with the addition of at least one compound of the formula (I) until homogeneous distribution.
  • active ingredients and auxiliaries of a photographic processing bath are mixed together with the addition of at least one compound of the formula (I) until homogeneous distribution.
  • This can be done by mechanical mixing in a conventional "Lödige mixer”, “Nauta mixer” or “Tumble dryer”, as well as by swirling air while spraying.
  • the formulations produced in this way are dust-free or low-dust, free-flowing, quick to dissolve, almost indefinitely durable and show no or minimal abrasion under mechanical stress, for example, assembly by means of dosing screws, but this is immediately bound again.
  • 1,000 g of potash are sprayed in an air vortex for 3.5 minutes with 20 g of a substance according to the invention or the specified amount of substance.
  • 1,000 g of potassium disulfite are mixed with 20 g of P 300 in a Lödige mixer for 5 minutes. The distribution is then homogeneous.
  • the color developer CD-4 is mixed with 1% by weight of P 600 (based on the total weight) in an eddy current for 3 minutes.
  • HX Hydroxylammonium sulfate
  • DTPA diethylenetriamine-pentaacetic acid

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Silver Salt Photography Or Processing Solution Therefor (AREA)
  • Detergent Compositions (AREA)

Abstract

In fester Form formulierte fotografische Verarbeitungschemikalien, enthaltend die erforderlichen Wirk- und Hilfsstoffe sowie zusätzlich wenigstens eine Verbindung der Formel (I), <IMAGE> worin R: C2-C4-Alkyl und; n: 1 - 200 bedeuten, oder wenigstens eine Verbindung der Formel, R1­OH (II) worin; R1: C10-C18-Alkyl bedeutet, oder wenigstens ein wasserlösliches Polymeres, z.B. aus der Reihe Polystyrolsulfonsäure und Polyvinylalkohol oder ein Gemisch wenigstens zweier vorgenannter Verbindungen, in einer Menge von 0,5 bis 100 g/kg Feststoff sind staubfrei oder staubarm.Photographic processing chemicals formulated in solid form, containing the required active substances and auxiliaries and additionally at least one compound of the formula (I), <IMAGE> in which R: C2-C4-alkyl and; n: 1 - 200, or at least one compound of the formula, R1OH (II) in which; R1: C10-C18-alkyl, or at least one water-soluble polymer, e.g. from the series polystyrene sulfonic acid and polyvinyl alcohol or a mixture of at least two of the aforementioned compounds, in an amount of 0.5 to 100 g / kg of solids are dust-free or low-dust.

Description

Die Erfindung betrifft in fester Form formulierte Fotochemikalien mit vermindertem Staubanteil und ein Verfahren zu ihrer Herstellung.The invention relates to solid-formulated photographic chemicals with a reduced dust content and a process for their production.

Fotografische Verarbeitungsbäder, z.B. Entwicklungs-, Bleich- und Fixierbäder enthalten die erforderlichen Wirkstoffe meist in geringer Konzentration und werden daher vom Benutzer aus Wasser und Chemikalienkonzentraten sowie gegebenenfalls weiteren Hilfsmitteln selbst angesetzt.Photographic processing baths, e.g. Developmental, bleaching and fixing baths usually contain the required active ingredients in low concentrations and are therefore prepared by the user himself from water and chemical concentrates as well as, if necessary, other auxiliaries.

Die Konzentrate sollen möglichst einfach zu dosieren und weitgehend staubfrei sein. Außerdem sollen für Verpackung und Transport keine unnötig hohen Kosten entstehen.The concentrates should be dosed as simply as possible and should be largely dust-free. In addition, no unnecessarily high costs should arise for packaging and transport.

Die in der Praxis allgemein üblichen Flüssigkonzentrate zur Herstellung gebrauchsfertiger fotografischer Bäder besitzen gegenüber den früher verwendeten, pulverförmig konfektionierten Produkten den Vorteil, daß keine Staubentwicklung und keine Lösungsprobleme auftreten. Die Konzentrate besitzen die Nachteile des hohen Gewichts- und Volumenanteils des Wassers, sowie Entsorgungsschwierigkeiten der unhandlichen Packmittel.The liquid concentrates which are generally used in practice for the production of ready-to-use photographic baths have the advantage over the previously used, powdered products that no dust development and no solution problems occur. The concentrates have the disadvantages of the high proportion by weight and volume of water, as well as difficulties in disposing of the bulky packaging.

Gemäß DE-OS 37 33 861 sprüh- oder gefriergetrocknete Produkte, die diese Nachteile vermeiden sollen, zeigen jedoch eine hohe Staubentwicklung.According to DE-OS 37 33 861 spray-dried or freeze-dried products which are intended to avoid these disadvantages, however, show a high level of dust.

Aufgabe der Erfindung ist daher, Mittel zu finden, mit denen in fester Form formulierte fotografische Verarbeitungschemikalien hergestellt werden können, deren Staubanteil vermindert ist, die also staubfrei oder zumindest staubarm sind. Die so hergestellten Produkte sollen sich darüber hinaus in kurzer Zeit in Wasser lösen.The object of the invention is therefore to find means with which photographic processing chemicals formulated in solid form can be produced, the dust content of which is reduced, and which are therefore dust-free or at least low-dust. The products manufactured in this way should also dissolve in water in a short time.

Es wurde nun gefunden, daß durch geringe Zusätze einer hydrophilen organischen Verbindung zu den festen Bestandteilen fotografischer Verarbeitungsbäder die gestellte Aufgabe gelöst werden kann.It has now been found that the object can be achieved by small additions of a hydrophilic organic compound to the solid components of photographic processing baths.

Als staubfrei bzw. staubarm werden solche Formulierungen bezeichnet, die frei von oder arm an Feststoffanteilen einer Korngröße <0,1 mm sind. Die Menge wird durch übliche Siebanalyse festgestellt; sie soll vorzugsweise unter 2 Gew.-%, insbesondere unter 1 Gew.-%, liegen.Formulations that are free of or low in solids with a grain size <0.1 mm are referred to as dust-free or low-dust. The amount is determined by conventional sieve analysis; it should preferably be below 2% by weight, in particular below 1% by weight.

Gegenstand der Erfindung sind daher in fester Form formulierte fotografische Verarbeitungschemikalien, enthaltend die erforderlichen Wirk- und Hilfsstoffe, dadurch gekennzeichnet, daß sie zusätzlich wenigstens eine Verbindung der Formel (I),

Figure imgb0001
worin

  • R C2-C4-Alkyl und
  • n 1 - 200 bedeuten, oder wenigstens eine Verbindung der Formel,
    Figure imgb0002
    worin
  • R1 C10-C18-Alkyl bedeutet,

oder wenigstens ein wasserlösliches Polymeres, z.B. aus der Reihe Polystyrolsulfonsäure und Polyvinylalkohol oder ein Gemisch wenigstens zweier vorgenannter Verbindungen,
in einer Menge von 0,5 bis 100 g/kg Feststoff, vorzugsweise von 5 bis 20 g/kg Feststoff, enthalten.The invention therefore relates to photographic processing chemicals formulated in solid form, containing the necessary active ingredients and auxiliaries, characterized in that they additionally contain at least one compound of the formula (I),
Figure imgb0001
 wherein
  • RC 2 -C 4 alkyl and
  • n is 1 to 200, or at least one compound of the formula
    Figure imgb0002
     wherein
  • R 1 is C 10 -C 18 alkyl,

or at least one water-soluble polymer, for example from the series polystyrene sulfonic acid and polyvinyl alcohol, or a mixture of at least two aforementioned compounds,
in an amount of 0.5 to 100 g / kg solid, preferably from 5 to 20 g / kg solid.

Geeignete Verbindungen der Formel 1 sind Ethylenglykol, Homologe des Ethylenglykols und Polyethylenglykole mit mittleren Molmassen von 200 bis 10.000 sowie Propylenglykol und Polypropylenglykole mit mittleren Molmassen von 200 bis 10.000, vorzugsweise Polyethylenglykole mit mittleren Molmassen von 300 bis 1.000, z.B. Polyethylenglykol 300, 400, 600 und 1.000; Kurzbezeichnung P 300, P 400, P 600, P 1000.Suitable compounds of formula 1 are ethylene glycol, homologues of ethylene glycol and polyethylene glycols with average molecular weights from 200 to 10,000 and propylene glycol and polypropylene glycols with average molecular weights from 200 to 10,000, preferably polyethylene glycols with average molecular weights from 300 to 1,000, e.g. Polyethylene glycol 300, 400, 600 and 1,000; Short designation P 300, P 400, P 600, P 1000.

Geeignete Verbindungen der Formel 11 sind Fettalkohole wie 1-Dodekanol oder Fettalkoholgemische, z.B. ein Gemisch mit gleichen Anteilen Ci2- und C, 4-Fettalkohol.Suitable compounds of the formula 11 are fatty alcohols such as 1-dodecanol or fatty alcohol mixtures, for example a mixture with equal proportions of C 2 and C 4 fatty alcohol.

Geeignete fotografische Verarbeitungschemikalien sind Schwarz-Weiß-Entwickler, Farbentwickler, Bleichmittel, Fixiermittel, Bleichfixiermittel und Stabilisiermittel.Suitable photographic processing chemicals are black and white developers, color developers, bleaching agents, fixing agents, bleach-fixing agents and stabilizers.

Diese fotografischen Verarbeitungschemikalien enthalten neben dem erfindungsgemäßen Zusatz die üblichen Wirk- und Hilfsstoffe. Einzelheiten dazu sind den Ausführungsbeispielen zu entnehmen.In addition to the additive according to the invention, these photographic processing chemicals contain the usual active substances and auxiliaries. Details can be found in the exemplary embodiments.

Das Verfahren zur Herstellung der erfindungsgemäßen entstaubten Produkte ist dadurch gekennzeichnet, daß man Wirk- und Hilfsstoffe eines fotografischen Verarbeitungsbades zusammen unter Zusatz wenigstens einer Verbindung der Formel (I) bis zur homogenen Verteilung mischt. Dies kann durch mechanisches Mischen in einem herkömmlichen "Lödige-Mischer", "Nauta-Mischer" oder "Taumeltrockner", sowie durch Luftverwirbelung unter gleichzeitigem Aufsprühen geschehen. Die so hergestellten Formulierungen sind staubfrei bzw. staubarm, rieselfähig, schnell löslich, nahezu unbegrenzt haltbar und zeigen bei mechanischer Beanspruchung, z.B. Konfektionierung mittels Dosierschnecken, keinen oder minimalen Abrieb, der aber sofort wieder gebunden wird.The process for the preparation of the dedusted products according to the invention is characterized in that active ingredients and auxiliaries of a photographic processing bath are mixed together with the addition of at least one compound of the formula (I) until homogeneous distribution. This can be done by mechanical mixing in a conventional "Lödige mixer", "Nauta mixer" or "Tumble dryer", as well as by swirling air while spraying. The formulations produced in this way are dust-free or low-dust, free-flowing, quick to dissolve, almost indefinitely durable and show no or minimal abrasion under mechanical stress, for example, assembly by means of dosing screws, but this is immediately bound again.

Es ist möglich und manchmal erforderlich, die einzelnen Bestandteile eines fotografischen Verarbeitungsbades getrennt nach dem erfindungsgemäßen Verfahren zu behandeln, dann miteinander zu mischen oder bis zur Ansetzung des Verarbeitungsbades getrennt zu halten; z.B. werden für ein farbfotografisches Entwicklungsbad Entwicklersubstanz, Alkalispender und Oxidationsschutzmittel getrennt behandelt und erst bei Ansatz der Entwicklerlösung vereinigt.Die übrigen Zusätze wie Kalkschutzmittel, Schwermetallkomplexbildner, Nariumsulfit und Alkalihalogenid können gemeinsam mit einem oder mehreren essentiellen Bestandteilen gemischt und behandelt werden.It is possible and sometimes necessary to treat the individual components of a photographic processing bath separately according to the process of the invention, then to mix them together or to keep them separate until the processing bath is prepared; e.g. developer substance, alkali dispenser and anti-oxidant are treated separately for a color photographic development bath and only combined when the developer solution is added.

Beispiel 1 (Staubbindung von Pottasche)Example 1 (Dust binding of potash)

1.000 g Pottasche werden im Luftwirbelstrom 3,5 min mit 20 g einer erfindungsgemäßen Substanz oder der angegebenen Menge an Substanz besprüht.

Figure imgb0003
Figure imgb0004
 1,000 g of potash are sprayed in an air vortex for 3.5 minutes with 20 g of a substance according to the invention or the specified amount of substance.
Figure imgb0003
Figure imgb0004

Beispiel 2 (Stabilisierbadregenerator)Example 2 (stabilizing bath regenerator)

Folgende Chemikalien werden mit 2 g P 600 im Wirbelstrom während 3 min besprüht:

Figure imgb0005
Figure imgb0006
 The following chemicals are sprayed with 2 g P 600 in an eddy current for 3 min:
Figure imgb0005
Figure imgb0006

Beispiel 3 (Kaliumdisulfit)Example 3 (Potassium Disulfite)

1.000 g Kaliumdisulfit werden mit 20 g P 300 in einem Lödige-Mischer 5 min vermischt. Die Verteilung ist danach homogen.

Figure imgb0007
1,000 g of potassium disulfite are mixed with 20 g of P 300 in a Lödige mixer for 5 minutes. The distribution is then homogeneous.
Figure imgb0007

Beispiel 4 (Bleichfixierbadregenerator)Example 4 (bleach-fix bath regenerator)

Folgende Chemikalien werden mit 0,5 Gew.-% P 600 (bezogen auf Gesamtfeststoff) in einem Taumeltrockner 5 min vermischt:

Figure imgb0008
The following chemicals are mixed with 0.5% by weight of P 600 (based on total solids) in a tumble dryer for 5 minutes:
Figure imgb0008

Beispiel 5 (Filmentwicklerregenerator)Example 5 (film developer regenerator) a) Alkaliteila) Alkali part

Folgende Chemikalien werden mit 2 Gew.-% P 600 (bezogen auf Gesamtfeststoff) im Wirbelstrom 3 min vermischt.

Figure imgb0009
Figure imgb0010
 The following chemicals are mixed with 2% by weight of P 600 (based on total solids) in an eddy current for 3 minutes.
Figure imgb0009
Figure imgb0010

b) Entwicklerteilb) developer part

Der Farbentwickler CD-4 wird mit 1 Gew.-% P 600 (bezogen auf Gesamtgewicht) im Wirbelstrom 3 min vermischt.

Figure imgb0011
The color developer CD-4 is mixed with 1% by weight of P 600 (based on the total weight) in an eddy current for 3 minutes.
Figure imgb0011

c) Hydroxylammoniumsulfat (HX)-Diethylentriamin-pentaessigsäure (DTPA)-Gemischc) Hydroxylammonium sulfate (HX) -diethylenetriamine-pentaacetic acid (DTPA) mixture

Folgende Substanzen werden im Wirbelstrom mit 1 Gew.-% P 600 (bezogen auf Gesamtgewicht) 3 min vermischt.

Figure imgb0012
The following substances are mixed in an eddy current with 1% by weight of P 600 (based on total weight) for 3 minutes.
Figure imgb0012

Claims (4)

1. In fester Form formulierte fotografische Verarbeitungschemikalien, enthaltend die erforderlichen Wirk-und Hilfsstoffe, dadurch gekennzeichnet, daß sie zusätzlich wenigstens eine Verbindung der Formel (I),
Figure imgb0013
worin R C2-C4-Alkyl und n 1 - 200 bedeuten, oder wenigstens eine Verbindung der Formel,
Figure imgb0014
worin R1 C10-C18-Alkyl bedeutet, oder wenigstens ein wasserlösliches Polymeres oder ein Gemisch wenigstens zweier vorgenannter Verbindungen, in einer Menge von 0,5 bis 100 g/kg Feststoff enthalten. 1. Photographic processing chemicals formulated in solid form, containing the required active ingredients and auxiliary substances, characterized in that they additionally contain at least one compound of the formula (I),
Figure imgb0013
 wherein RC 2 -C 4 alkyl and n is 1 to 200, or at least one compound of the formula
Figure imgb0014
 wherein R 1 is C 10 -C 18 alkyl, or at least one water-soluble polymer or a mixture of at least two aforementioned compounds, contained in an amount of 0.5 to 100 g / kg of solid. 2. In fester Form formulierte fotografische Verarbeitungschemikalien nach Anspruch 1, dadurch gekennzeichnet, daß sie weniger als 2 Gew.-% an Feststoffanteilen einer Korngröße <0,1 mm aufweisen.2. Photographic processing chemicals formulated in solid form according to claim 1, characterized in that they have less than 2 wt .-% of solids with a grain size <0.1 mm. 3. In fester Form formulierte fotografische Verarbeitungschemikalien nach Anspruch 1, dadurch gekennzeichnet, daß sie wenigstens ein Polyethylenglykol mit mittlerer Molmasse von 300 bis 1000 enthalten.3. Photographic processing chemicals formulated in solid form according to claim 1, characterized in that they contain at least one polyethylene glycol with an average molecular weight of 300 to 1000. 4. In fester Form formulierte fotografische Verarbeitungschemikalien nach Anspruch 1, dadurch gekennzeichnet, daß sie die zusätzliche Verbindung in einer Menge von 0,5 bis 100 g/kg Feststoff enthalten.4. Photographic processing chemicals formulated in solid form according to claim 1, characterized in that they contain the additional compound in an amount of 0.5 to 100 g / kg of solid.
EP91112641A 1990-08-11 1991-07-27 Photographic chemicals with reduced dust fraction Expired - Lifetime EP0472007B1 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE4025560 1990-08-11
DE4025560A DE4025560A1 (en) 1990-08-11 1990-08-11 PHOTO CHEMICALS WITH REDUCED STAUBANT

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EP0472007A1 true EP0472007A1 (en) 1992-02-26
EP0472007B1 EP0472007B1 (en) 1997-02-05

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JP (1) JP2904969B2 (en)
DE (2) DE4025560A1 (en)

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EP0638843A2 (en) * 1993-07-29 1995-02-15 Konica Corporation Solid processing agent for silver halide photographic light-sensitive materials
US5460937A (en) * 1993-10-20 1995-10-24 Eastman Kodak Company Process for incorporating a hydrophobic compound into an aqueous medium

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JPH07295162A (en) 1994-04-28 1995-11-10 Konica Corp Solid processing agent for silver halide photographic sensitive material
EP0687951B1 (en) * 1994-06-10 2001-10-10 Konica Corporation Granular or tablet-form color-developing composition
JPH0990573A (en) * 1995-09-28 1997-04-04 Konica Corp Solid developing replenisher for processing silver halide photographic sensitive material and developing method using the same
US5900355A (en) * 1998-03-26 1999-05-04 Eastman Kodak Company Method of making uniformly mixed dry photographic processing composition using hot melt binder
DE60018376T2 (en) * 1999-12-27 2005-07-21 Fuji Photo Film Co., Ltd., Minami-Ashigara Solid granulated processing agent for silver halide photographic material and its method of preparation

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Publication number Priority date Publication date Assignee Title
WO1994011783A1 (en) * 1992-11-13 1994-05-26 Sun Chemical Corporation Solid antifoggant agent and solid single part high contrast rapid access developer
EP0638843A2 (en) * 1993-07-29 1995-02-15 Konica Corporation Solid processing agent for silver halide photographic light-sensitive materials
EP0638843A3 (en) * 1993-07-29 1996-03-06 Konishiroku Photo Ind Solid processing agent for silver halide photographic light-sensitive materials.
US5460937A (en) * 1993-10-20 1995-10-24 Eastman Kodak Company Process for incorporating a hydrophobic compound into an aqueous medium

Also Published As

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DE59108527D1 (en) 1997-03-20
JP2904969B2 (en) 1999-06-14
JPH04254853A (en) 1992-09-10
EP0472007B1 (en) 1997-02-05
DE4025560A1 (en) 1992-02-13
US5258268A (en) 1993-11-02

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