Radiation imagery chemistry: process – composition – or product th – Radiation sensitive product – Silver compound sensitizer containing
Reexamination Certificate
2000-06-23
2002-04-23
Chea, Thorl (Department: 1752)
Radiation imagery chemistry: process, composition, or product th
Radiation sensitive product
Silver compound sensitizer containing
C554S074000
Reexamination Certificate
active
06376168
ABSTRACT:
TECHNICAL FIELD
The present invention relates to a method for preparing fatty acid silver salt and a heat-developable photosensitive material incorporating the fatty acid silver salt obtained by such preparation method.
RELATED ART
A strong need for reducing the volume of waste process solution has arisen in recent medical field from viewpoints of environmental preservation and space saving. Thus a technology related to a photosensitive heat-developable photographic material for medical diagnosis and photographic purposes has been desired, the material being such that affording efficient light exposure with a laser image setter or laser imager, and providing a black image with high resolution and sharpness. Such photosensitive heat-developable photographic material can provide the user with a more simple and environment-conscious image producing system using no solution-base process chemicals.
The image producing method based on heat development is disclosed, for example, in U.S. Pat. Nos. 3,152,904 and 3,457,075 and “Thermally Processed Silver Systems” written by D. Morgan and B. Shely, Imaging Processes and Materials, Neblette's 8th ed., edited by Sturge, V. Walworth and A. Shepp, p.2, (1989).
Such photosensitive material contains an organic reducible non-photosensitive silver source (e.g., organic acid silver salt), a catalytic amount of photocatalyst (e.g., silver halide) and a reducing agent for silver, all of which being generally dispersed in an organic binder matrix. While the photosensitive material is stable at the room temperature, it will produce silver through a redox reaction between the reducible silver source and the reducing agent when heated to a high temperature (80° C. or above, for example) after light exposure. The redox reaction is promoted by a catalytic action of the latent image produced by the light exposure. That is, the silver generated by the reaction of the reducible silver within the exposed area provides a black spot, which makes a contrast with the non-exposed area and is recognizable as an image.
The silver source employed by such system generally refers to a silver salt of a fatty acid, and a variety of methods for producing thereof have been known. Examples of the methods include such that preparing an organic acid silver salt in a concomitant solution of water and water-insoluble solvent as disclosed for example in JP-A-49-93310 (the code “JP-A” as used herein means an “unexamined published Japanese patent application”), JP-A-49-94619 and JP-A-53-68702; such that preparing an organic acid silver salt in an aqueous solution as disclosed in JP-A-53-31611, JP-A-54-4117 and JP-A-54-46709; such that preparing an organic acid silver salt in an organic solvent as disclosed in JP-A-57-186745, JP-A-47-9432 and U.S. Pat. No. 3,700,458. In principle, the organic acid silver salt is obtained by dissolving a fatty acid into water under heating to a temperature of the melting point thereof or above, adding sodium hydroxide or an alkali metal salt under vigorous stirring, and further adding silver nitrate to convert an alkali soap into a silver soap.
The alkali soap forms micell in the aqueous solution, which appears as a milky liquid. The conversion reaction from such micellar state to silver salt, however, often suffers from a problem in production stability. Thus as a measure for obtaining a homogeneous solution of alkali soap, use of a mixed solution of water and alcohol as a solvent is disclosed in JP-A-55-40607.
Now the alkali soap shows alkalinity as its name suggests, and is prepared under a high pH environment. Adding silver nitrate to an alkali solution, however, not only produces silver oxide as a by-product but also results in an undesirable production of silver nucleus by an action of a trace amount of contaminant which inevitably generates during the production and exhibits a high reducing activity under such high-pH environment. Such by-product is quite disadvantageous in that degrading property of the heat-developable photographic material and in particular in that causing undesirable fog. From this viewpoint, a method for obtaining a homogeneous solution to suppress the generation of the by-product is disclosed in JP-A-55-40607, in which fog still remains unsolved.
In JP-A-9-127643, disclosed is a method for producing silver salt based on simultaneous measuring and addition of an alkali metal salt solution and silver nitrate solution, and is specified as simultaneous addition of aqueous sodium behenate solution and isopropyl alcohol. While the method is successful in at least lowering the high pH during the reaction to the medium range and thereby in suppressing the generation amount of silver oxide, fog still cannot totally be cleared due to a weak reducibility of isopropyl alcohol.
As described above, preparation of fatty acid silver salt needs special accounts such that eliminating as possible reducible substances during the formation of fatty acid silver salt, controlling the grain size and controlling the grain form, where all of them cannot be satisfied at a time by the conventional method.
In the production of a heat-developable photosensitive material using the fatty acid silver salt, a photosensitive layer thereof is often formed by coating a coating liquid containing an organic solvent such as toluene, methyl ethyl ketone or methanol. Using an organic solvent as the solvent, however, is not only disadvantageous in terms of safety in the production processes, adverse effects on human body, and high cost ascribable to the solvent recovery or the like, but is also inappropriate in terms of providing an environment-conscious heat-developable photosensitive material.
Thus a method for forming the photosensitive layer using a water-base coating liquid. For example, JP-A-49-52626 and JP-A-53-116144 disclose cases using gelatin as a binder. In JP-A-50-151138, a case using polyvinyl alcohol as a binder is described.
A case with a combined use of gelatin and polyvinyl alcohol is found in JP-A-60-61747. As another exemplary case, the photosensitive layer using a water-soluble polyvinyl acetal as a binder is described in JP-A-58-28737.
As is clear from the above, using a water-soluble binder allows the photgosensitive layer to be formed with awater-base coating liquid and is beneficial from environmental and economic viewpoints. The water-soluble polymer binder is, however, less compatible with the fatty acid silver salts, which will fail in obtaining a coated film with a surface quality agreeable to the practical use, will result in brownish to yellowish tone of the silver image after the development afar from intrinsically preferable black tone and will result in increased fog. Thus only afforded was a heat-developable photosensitive material whose property being significantly degraded and commercially unsuccessful.
In order to obtain practically agreeable quality of the coated surface using the water-base coating liquid containing a fatty acid silver salt, the fatty acid silver salt must be kept in a finely dispersed state in the water-base solution without agglomeration. Discovery of a method for finely dispersing the fatty acid silver salt is thus desired. One method generally accepted relates to such that producing a hydrophobic grain dispersion of a fatty acid silver salt, separating the grain therefrom by filtration to obtain a solid matter, and re-dispersing the solid matter after being mixed with a dispersing agent as described by D. Kloosterboer in Imaging Processes and Materials, Neblette's 8th ed., edited by Sturge, V. Walworth and A. Shepp, p.279, (1989).
Fine dispersion operation of the fatty acid silver salt can be effected by mechanical dispersion in the presence of a dispersing agent using a known pulverizing means (e.g., high-speed mixer, homogenizer, high-speed impact mill, banbury mixer, homomixer, kneader, ball mill, vibration ball mill, epicyclic ball mill, attritor, sand mill, bead mill, colloid mill, jet mill, roller mill, trommel and high-speed stone mill). These methods, however, produce only a coating
Chea Thorl
Fuji Photo Film Co. , Ltd.
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