US2271176A - Process for the manufacture of color photographic images - Google Patents

Process for the manufacture of color photographic images Download PDF

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Publication number
US2271176A
US2271176A US309300A US30930039A US2271176A US 2271176 A US2271176 A US 2271176A US 309300 A US309300 A US 309300A US 30930039 A US30930039 A US 30930039A US 2271176 A US2271176 A US 2271176A
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Prior art keywords
acid
solution
silver
layer
dye
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Expired - Lifetime
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US309300A
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English (en)
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Gaspar Bela
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Chromogen Inc
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Chromogen Inc
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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
    • G03C7/00—Multicolour photographic processes or agents therefor; Regeneration of such processing agents; Photosensitive materials for multicolour processes
    • G03C7/26—Silver halide emulsions for subtractive colour processes

Definitions

  • a known process for the manufacture of colorphotographic images and more specifically for the conversion of a negative silver image into a positive dye-image consists in treating a film containing a silver image and diffusely dyed with an aio-dye in a dilute solution of a hydrohalic acid, whereby the dyestufi is bleached out at the places where silver is present. It is also known to produce diffusely dyed photographic layers or films by building up an azodyestuff from a diazo-compound and an azo-coupler within the layer or the emulsion used for its preparation such, for example, as is disclosed in my Letters Patent 2,071,688 dated February 23, 1937.
  • the photographic layer is washed for a short time and then treated in an alkaline solution containing sufficient alkali, such'for example, as sodium carbonate to insure an alkaline reaction. Coupling of the azo-coupler and the portion of the diazo-compound present which was not previously destroyed takes place in this alkaline solution to complete the formation of the dye images.
  • alkali such'for example, as sodium carbonate
  • Various substances may be used to prepare the acid solution described above, among which are hydrohalic acids and other dye-destroying baths" of acidic reaction which are described in my Letters Patent 2,020,775 dated November 12, 1935.
  • Such acid solutions are used in a concentration at which coupling does not occur.
  • a 3-12% hydrochloric acid or a 2-10% hydrobromic acid may be used for this purpose.
  • the concentration of acid which has been found effective to prevent coupling of most of the diazo-compounds has a pH range in the vicinity of 2 to 3 although this concentration may be increased or decreased, especially if catalysts such as dimethyl-quinoxaline are added to the acid solution.
  • Example I.A- light sensitive silver halide emulsion layer is treated for fifteen minutes in a bath containing 0.5 g. of B-naphthol and 0.5 g. caustic soda in cos. of water, washed, and dried. The layer is exposed, developed and fixed in the usual manner. Instead of impregnating the layer with the B-naphthol before the exposure, the impregnation may also be efiected with the exposed and developed layer containing the silver image. The layer is thereupon treated for two minutes at +5 C. with a solution containing 5% hydrobromic acid and 1% diazotized a-naphthylamine.
  • the layer After a short washing the layer is immersed in a 2N aqueous sodium carbonate solution, washed again, treated in a copper chloride solution and fixed out. In this manner an insoluble magenta dye is formed in inverse proportion to the amount of silver present.
  • Example II Instead of using 5% hydrobromic acid in the above example, the following may be substituted:
  • Example III Instead of using B-naphthol as set forth in Examples I and II above, 2-oxy-3- naphthoylanilide may be employed. Substitution of 2-oxy-3-naphthoylanilide in the above examples will result in an insoluble purple dye.
  • Example IV The light sensitive silver halide emulsion layer containing the p-naphthol as set forth in Examples I and II may be treated for 1% minutes at 18 C. in 20 cos. of 11% aqueous hydrochloric acid solution containing diazotized diamino-stilbene disulphonic acid.
  • This bath may beprepared by dissolving 0.37 g. of diaminostilbene sulphonic acid in 20 cos. of aqueous hydrochloric acid and diazotising by the addition of 0.18 g. of sodium nitrite.
  • a violet dye is obtained at the places where no silver was present.
  • an acid or neutral developer is used instead of the alkaline developer.
  • an acid or neutral developer is used instead of the alkaline developer.
  • an inorganic acid or neutral developer may be em ployed.
  • the following developer for example, is suitable.
  • Solution 1 100 grms. potassium oxalate dissolved in 400 cos. of water.
  • Solution 2 100 grms. ferrous sulphate and l grm. citric acid dissolved in 300 cos. of water.
  • the film is washed for a short time, immersed in a 2n sodium carbonate solution, washed again, treated in a copper chloride solution and fixed out. In this manner a magenta dye is obtained at the places where no silver was present.
  • Example VI A film containing a silver image and impregnated with fl-naphtol as described in Example I, is treated 3 minutes at 18 C. in a solution prepared in the following manner. 11.9 grms. potassium bromide and 2.8 cos. of conc. sulfuric acid are dissolved in water to form 100 ccs. 0.68 grm. Diazolichtgelb 3 GL (Schultz Farbstofftabellen, 7th ed., supplement I, page 87) are dissolved in 20 cos. of this solution and then 0.18 grm. of sodium nitrite are added. After the treatment in this solution the film is washed for a short time, immersed in 2n sodium carbonate solution, washed again, treated in a copper chloride solution and fixed out. In this manner an orange dye is obtained at the places where no silver was present.
  • Emample VII .--A film containing a silver image and impregnated with s-naphtol as described in Example I, is treated'3 minutes at 18 C. in a solution prepared in the following manner. 11.9 grms. potassium bromide and 2.8 cos. of cone. sulfuric acid are dissolved in water to form 100 C05. 0.57 grm. Primuline (Schultz, Farbstofltabellen, 7th ed., vol. I, No. 932) are dissolved in 20 cos. of this solution and then 0.09 grm. sodium nitrite are added.
  • the improved process described above is suitable to form multi-color images in a multilayer material having different dye coupling components and different silver part images in superimposed layers, such as described in Letters Patent 2,166,049 which issued to me July 11, 1939.
  • the process of producing a photographic dye-image which comprises exposing a photographic silver halide emulsion layer uniformly impregnated with an azo-dye coupler, developing said layer and treating said layer with a diazonium salt in a hydrohalic acid solution, which has a pI-I-value at which coupling does not occur but at which said solution reacts with the silver to produce a reaction product whereby the coupling property of the diazonium salt is locally destroyed at the points of silver deposit by reduction, thereafter neutralising said acid within ing said layer with a developer having neutral to acid character and treating said layer with a diazonium salt in a hydrohalic acid solution which has a pH-value at which coupling does not occur but at which said solution reacts with the silver to produce a reaction product whereby the coupling property of the diazonium salt is locally destroyed at the points of silver deposit by reduction, thereafter neutralising said acid withinsaid layer sufliciently to cause said amcoupler to combine with said diazonium compound and removing the silver

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  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Non-Silver Salt Photosensitive Materials And Non-Silver Salt Photography (AREA)
US309300A 1938-12-19 1939-12-14 Process for the manufacture of color photographic images Expired - Lifetime US2271176A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2681856A (en) * 1949-04-04 1954-06-22 Gaspar Photographic material and process for making an azo dye bleachout image
US2688542A (en) * 1949-02-09 1954-09-07 Bela Gaspar Material and process for the production of color photographic images
US2778813A (en) * 1951-05-08 1957-01-22 Gaspar Color photographic material from resinous sulfonyl chlorides
US3338711A (en) * 1962-11-15 1967-08-29 Du Pont Process for forming azo dye photographic images
US3340059A (en) * 1963-02-27 1967-09-05 Du Pont Diffusion transfer process for producing silver-free azo dye images

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2688542A (en) * 1949-02-09 1954-09-07 Bela Gaspar Material and process for the production of color photographic images
US2681856A (en) * 1949-04-04 1954-06-22 Gaspar Photographic material and process for making an azo dye bleachout image
US2778813A (en) * 1951-05-08 1957-01-22 Gaspar Color photographic material from resinous sulfonyl chlorides
US3338711A (en) * 1962-11-15 1967-08-29 Du Pont Process for forming azo dye photographic images
US3340059A (en) * 1963-02-27 1967-09-05 Du Pont Diffusion transfer process for producing silver-free azo dye images

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