EP1003077B1 - Procédé de fabrication de produits chimiques photographiques sous forme de comprimé - Google Patents

Procédé de fabrication de produits chimiques photographiques sous forme de comprimé Download PDF

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Publication number
EP1003077B1
EP1003077B1 EP99119025A EP99119025A EP1003077B1 EP 1003077 B1 EP1003077 B1 EP 1003077B1 EP 99119025 A EP99119025 A EP 99119025A EP 99119025 A EP99119025 A EP 99119025A EP 1003077 B1 EP1003077 B1 EP 1003077B1
Authority
EP
European Patent Office
Prior art keywords
weight
tablet
tablets
hardness
raw materials
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
EP99119025A
Other languages
German (de)
English (en)
Other versions
EP1003077A2 (fr
EP1003077A3 (fr
Inventor
Axel Dr. Hengefeld
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.)
Tetenal Photowerk & Co GmbH
Original Assignee
Tetenal Photowerk & Co GmbH
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Tetenal Photowerk & Co GmbH filed Critical Tetenal Photowerk & Co GmbH
Publication of EP1003077A2 publication Critical patent/EP1003077A2/fr
Publication of EP1003077A3 publication Critical patent/EP1003077A3/fr
Application granted granted Critical
Publication of EP1003077B1 publication Critical patent/EP1003077B1/fr
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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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
    • 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 a method for manufacturing of photographic formulated as tablets (especially tablets) Process chemicals and those obtainable by these processes corresponding moldings.
  • Exposed silver halide films are made in commercial laboratories developed and processed fully automatically. Color negative films for example, run through a developer bath Bleaching bath, a fixing bath and usually a stabilizing bath or several washing steps. The steps of bleaching and Fixing can be done using a bleach-fixing bath in one single processing step can be combined. The done developed negatives are exposed on color paper, the exposed color paper then also runs through a development bath, usually a combined bleach-fix bath and final washing steps. The washing steps can be replaced by a stabilizing bath if necessary.
  • Liquid concentrates need due to their water content Transport and storage a relatively large amount of space.
  • the empty ones Concentrate containers represent a considerable volume of waste.
  • Powdered chemicals are difficult to handle. Since the Precautions must be taken if powder can become dusty during handling to avoid adverse health effects for users to be hit.
  • EP-A 0 611 986 discloses solid photographic process chemicals. The chemicals are first granulated and then closed Tablets pressed.
  • the granulation of the process chemicals before pressing one tablet is expensive.
  • the object of the invention is to achieve this based on a simple, inexpensive method of manufacture to create such moldings.
  • a shaped body is any body with one through shaping purposefully manufactured shape. It is preferably around a tablet.
  • Photographic process chemicals are any chemicals that as part of one or more photographic processes (e.g. developing, fixing, bleach-fixing or the like) Can find application.
  • the input materials are all those Substances that are part of the molded body. It is about on the one hand about the person or persons in the respective photographic Processing process of active substances (e.g. fixing and / or Bleach-fixing agent, developer) and auxiliary substances, which are photographically inert or conducive to photography.
  • active substances e.g. fixing and / or Bleach-fixing agent, developer
  • auxiliary substances which are photographically inert or conducive to photography.
  • All of the insert materials of the molded body are preferably water-soluble.
  • a tablet produced according to the invention dissolves when setting the usual concentrations of the process chemicals completely in aqueous solution at the usual bath temperatures where the solution process can be slow, if such a tablet, for example, to regenerate a process bath serves. Any auxiliaries must be in such Extent be water soluble that dissolving for adjustment the desired concentration is not hindered.
  • auxiliary substances that are photographically beneficial can be buffer substances, for example to set a desired pH, water softener (in particular complexing agents), possibly optical Brighteners, preservatives, antioxidants, antifoggants, Solubilizers, emulsifiers and additives to increase resistance to moisture his.
  • water softener in particular complexing agents
  • optical Brighteners preservatives
  • antioxidants antioxidants
  • antifoggants Solubilizers
  • emulsifiers and additives to increase resistance to moisture his.
  • An exemplary disclosure of suitable auxiliaries can be found in DE-A-197 46 879. Reference is also made to the disclosure in Ullmanns Encyclopedia Chemicals Industrial Chemistry, 5th edition, vol. A20, chapter "Photography".
  • Auxiliaries include, for example, photographic inert adjuvants for tableting in question. It can be fillers, Binders, lubricants, flow regulators, lubricants, Act mold release agents and the like. For definition the terms and for an exemplary list suitable additives are referred to Rudolf Voigt, Textbook of Pharmaceutical Technology, 5th ed., Verlag Chemie, Weinheim 1984, page 178 ff.
  • At least 50% of the inorganic portion of the feed materials is crushed to an average grain size of 125 ⁇ m or less.
  • the comminution can be carried out by any suitable method, preferably the corresponding proportion of the feed materials is ground.
  • the average grain size ⁇ m is defined according to DIN 66141 (page 18) by: Q3 i represents the mass distribution, the proportion of a grain class to the associated grain class.
  • the feed materials are pressed directly (Direct tabletting) to a shaped body with a Molded hardness of at least 400 N.
  • direct pressing or direct tabletting refers to the compression of powdery feedstocks without one over the invention Pre-treatment to a size reduction Moldings.
  • Pre-treatment to a size reduction Moldings means "Direct pressing" that in any case that portion of the feed materials that in step a) to the specified grain size is crushed, no further pretreatment, in particular no granulation (e.g. fluidized bed granulation) is subjected.
  • no granulation e.g. fluidized bed granulation
  • the invention should not be excluded be that a remaining portion of the input materials (e.g. possible organic components) of a pretreatment such as Undergoes granulation. It is preferred according to the invention however, if all feed materials are not pretreated undergo, but immediately as a powder of Undergo direct tableting.
  • the molded article produced according to the invention has a hardness from at least 400 N.
  • the hardness is measured with a breaking strength tester TBH30 from ERWEKA.
  • the tablet to be tested is between two extendable jaws clamped and with one rising Force applied.
  • the one required to break the tablet Force is registered (in N) and as a measure of the Tablet hardness specified.
  • the moldings produced according to the invention preferably have an abrasion of less than 2%, more preferably less than 1%.
  • This abrasion or the abrasion resistance is measured according to that in Example 3 of the present application specified procedures.
  • the invention has recognized that surprisingly hard and sufficient abrasion-resistant tablets that are suitable for use in automatic feed magazines of commercial development machines are suitable, thanks to the direct compression without any need a complex pretreatment of at least one essential Manufacture proportion of the ingredients of the tablet to let.
  • This is surprising given the state of the art (Rudolf Voigt, textbook of pharmaceutical technology, Page 154 ff.) Teaches that when pressing directly, it becomes finer Do not manufacture powder tablets of sufficient strength to let. It is expressly stated there that the Direct tabletting, at most, coarse crystalline substances grain sizes between 0.5 and 1 mm are considered optimal designated.
  • the invention has recognized that contrary this teaching of the prior art hard and abrasion resistant Tablets can be made by direct compression correspondingly fine powder.
  • At least 70% by weight is more preferred at least 80% by weight, more preferably at least 90% by weight of the inorganic portion of the feed materials crushed to the specified grain sizes.
  • the invention can be the total inorganic portion of the feed materials can be comminuted accordingly, and any one organic part in whole or in part in this crushing be included.
  • the moldings can contain binders, but their proportion preferably below 10% by weight, more preferably below 5, is less than 2 or less than 1% by weight. Possibly. can on binder to be completely dispensed with.
  • At least 50% by weight are preferred, more preferably at least 80% by weight, more preferably at least 90 or 95 %
  • ammonium and or sodium thiosulfate are examples of the raw materials inorganic substances.
  • the tablets produced according to the invention with these salts as the main component for example Use in a fixer or bleach-fixer his.
  • ammonium thiosulfate 90/10 which is 90% commercially available consists of ammonium thiosulfate and 10% sodium thiosulfate, were in a BAUERMEISTER powder mill with turbo insert ground to a particle size of less than 125 ⁇ m.
  • the degree of pulverization was 90%.
  • the degree of pulverization was 100%, ie the main inorganic component was used completely pulverized.
  • the three mixtures were each 9.7 g of sodium N-lauroyl sarcosinate, that as a lubricant and lubricant Tableting is used, added and for 10 min until receipt mixed into a homogeneous mixture.
  • Tablet breaking strength 6 tablets in each case were tested for breaking strength using a TBH 30 tablet breaking strength tester from ERWEKA and the mean value was formed. A hardness of> 400 N is required to avoid damage during transport.
  • the powder mixture is granulated in the fluidized bed, then dried at an air temperature of 60 ° C for 8 min and finally at an air temperature of 0 ° C within 7 min cooled to 35 ° C.
  • the entire fluidized bed granulation process was complete after 1 h 25 min.
  • Example 1 the individual powder mixtures were pressed into tablets.
  • the tablets had the breaking strengths given in Table 3: Degree of powdering ammonium thiosulfate 90/10 44.4% (not according to the invention) 90% 100% Tablet hardness [N] Tablet hardness [N] Tablet hardness [N] maltodextrin 229 408 657 Sokalan CP45 305 474 856 Luvitec VPI 55 K18P 368 607 828 Luviskol K90 346 545 754 D-sorbitol 352 541 806 D-mannitol 305 415 759 Sorbitol / xylitol 351 517 751
  • Tablet abrasion Five tablets are weighed and placed in the plexiglass drum of an ERWEKA TA-10 tablet abrasion and friability tester. After a rotation time of 5 minutes, the tablets are freed of adhering dust and weighed again. The percentage abrasion is calculated from the weight loss in relation to the initial weight.
  • Example 3 Average of 6 tablets Comparative Example 2 Average of 6 tablets After 0 days Tablet thickness [mm] 9.50 9.46 Tablet hardness [N] 509 459 Tablet abrasion [%] 0.50 0.20 After 14 days at 50 ° C Tablet thickness [mm] 9.63 9.57 Tablet hardness [N] 639 672 After 28 days at 50 ° C Tablet thickness [mm] 9.57 9.80 Tablet hardness [N] 661 408
  • the cooled melt granulate was treated with 67.35 kg of ammonium thiosulfate 90/10, which had previously been ground in a BAUERMEISTER powder mill with turbo insert to a particle size of ⁇ 125 ⁇ m, with 5.03 kg of sodium disulfite, 9.25 kg of sodium sulfite, 410 g Maltodextrin and 1.46 kg of sodium N-lauroyl sarcosinate mixed in a mixer for 10 minutes to a homogeneous mass.
  • the final blend obtained was compressed on a rotary tablet press of the FETTE 2090 type to tablets with a diameter of 30 mm and a weight of 10.73 g.
  • Example 4 Average of 6 tablets Comparative Example 3 Average of 6 tablets After 0 days Tablet thickness [mm] 9.58 10.08 Tablet hardness [N] 489 828 Tablet abrasion [%] 0.45 0.37 After 7 days at 50 ° C Tablet thickness [mm] 9.68 10.10 Tablet hardness [N] 728 868 After 14 days at 50 ° C Tablet thickness [mm] 9.70 10.11 Tablet hardness [N] 740 818

Landscapes

  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Detergent Compositions (AREA)
  • Crushing And Pulverization Processes (AREA)
  • Medicinal Preparation (AREA)

Claims (7)

  1. Procédé de fabrication de produits chimiques de processus photographiques formulés en tant que corps moulé, comportant les étapes suivantes :
    a) Broyage d'au moins 50 % en poids de la fraction inorganique des matériaux mis en oeuvre à une granulométrie de 125 µm ou inférieure,
    b) Compression directe des matériaux mis en oeuvre en un corps moulé d'une dureté minimale de 400 N.
  2. Procédé selon la revendication 1, caractérisé en ce qu'au moins 70 % en poids, de préférence au moins 80 % en poids de la fraction inorganique des matériaux mis en oeuvre sont broyés à une granulométrie moyenne de 125 µm ou inférieure.
  3. Procédé selon revendication 1 ou 2, caractérisé en ce que les matériaux mis en oeuvre contiennent des excipients solubles dans l'eau, photographiquement inertes et/ou photographiquement utiles.
  4. Procédé selon la revendication 3, caractérisé en ce que les matériaux mis en oeuvre contiennent des liants.
  5. Procédé selon la revendication 4, caractérisé en ce que la fraction de liant est inférieure à 10 % en poids, de préférence inférieure à 5 % en poids, plus préférablement inférieure à 2 % en poids, encore plus préférablement à 1 % en poids.
  6. Procédé selon l'une quelconque des revendications 1 à 5, caractérisé en ce qu'au moins 50 % en poids, de préférence au moins 80 % en poids, plus préférablement au moins 90 % en poids, encore plus préférablement au moins 95 % en poids des matériaux mis en oeuvre sont des substances inorganiques.
  7. Procédé selon l'une quelconque des revendications 1 à 6 pour la fabrication d'un corps moulé à utiliser dans un bain de fixage ou un bain de fixage et de blanchiment.
EP99119025A 1998-11-18 1999-09-29 Procédé de fabrication de produits chimiques photographiques sous forme de comprimé Expired - Lifetime EP1003077B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE19853273 1998-11-18
DE19853273A DE19853273A1 (de) 1998-11-18 1998-11-18 Verfahren zur Herstellung von als Tablette formulierten fotografischen Prozeßchemikalien

Publications (3)

Publication Number Publication Date
EP1003077A2 EP1003077A2 (fr) 2000-05-24
EP1003077A3 EP1003077A3 (fr) 2000-09-20
EP1003077B1 true EP1003077B1 (fr) 2004-01-07

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Family Applications (1)

Application Number Title Priority Date Filing Date
EP99119025A Expired - Lifetime EP1003077B1 (fr) 1998-11-18 1999-09-29 Procédé de fabrication de produits chimiques photographiques sous forme de comprimé

Country Status (2)

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EP (1) EP1003077B1 (fr)
DE (2) DE19853273A1 (fr)

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0160087A4 (fr) * 1983-10-24 1987-06-29 Basf Wyandotte Corp Procede de preparation de poudres sechees par pulverisation contenant une vitamine soluble dans l'eau et poudres ainsi preparees.
EP0611986A1 (fr) * 1993-02-15 1994-08-24 Konica Corporation Composition solide de traitement photographique pour matériau photographique couleur à l'halogénure d'argent sensible à la lumière
DE69520079T2 (de) * 1994-04-19 2001-06-21 Konishiroku Photo Ind Herstellungsverfahren für feste Verarbeitungszusammensetzungen für photographische, lichtempfindliche Silberhalogenidmaterialien

Also Published As

Publication number Publication date
EP1003077A2 (fr) 2000-05-24
DE19853273A1 (de) 2000-05-25
EP1003077A3 (fr) 2000-09-20
DE59908242D1 (de) 2004-02-12

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