EP0687951B1 - Farbentwicklungszusammensetzung in Granulat- oder Tablettenform - Google Patents

Farbentwicklungszusammensetzung in Granulat- oder Tablettenform Download PDF

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Publication number
EP0687951B1
EP0687951B1 EP95303857A EP95303857A EP0687951B1 EP 0687951 B1 EP0687951 B1 EP 0687951B1 EP 95303857 A EP95303857 A EP 95303857A EP 95303857 A EP95303857 A EP 95303857A EP 0687951 B1 EP0687951 B1 EP 0687951B1
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EP
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Prior art keywords
solid processing
processing composition
tablet
molecular weight
average molecular
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EP95303857A
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English (en)
French (fr)
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EP0687951A1 (de
Inventor
Takashi Deguchi
Ichiro Tsuchiya
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Konica Minolta Inc
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Konica Minolta 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
    • 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
    • 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
    • G03C7/30—Colour processes using colour-coupling substances; Materials therefor; Preparing or processing such materials
    • G03C7/407—Development processes or agents therefor
    • G03C7/413—Developers

Definitions

  • the present invention relates to a granular processing composition and to a process for preparing a solid processing composition in the form of a tablet (hereinafter, granular and tablet forms are referred to simply as a solid processing composition as a general term) both for color-developing a silver halide color photographic light-sensitive material.
  • Japanese Patent O.P.I. Publication No. 119450/1993 there is disclosed a tablet whose moisture content is controlled to 0.5 - 10.0 wt%.
  • a tablet made by this method is greatly improved in residue rate of a color developing agent, in the state of a tablet immediately after it is dropped, and in the presence of insoluble material. Even in this method, however, there is a new problem in that the solid processing composition may swell or causes blocking.
  • the tablet made through this method is remarkably improved, as compared with a conventional tablet, in dissolving property, residue rate of paraphenylenediamine type color developing agent, reduction of occurrence of insoluble material and strength as well as molding property of the tablet.
  • an object of the invention is to provide a granular processing composition and a process for preparing a tablet-form processing composition used for preparing a color-developing solution for a silver halide color photographic light-sensitive material capable of greatly reducing generation of fine powder caused by hygroscopic swelling of a solid processing composition.
  • Another object of the invention is to provide a granular solid processing composition and a process for preparing a tablet-form processing composition used for colour-developing a silver halide colour photographic light-sensitive material wherein the problem of sticking together of the solid processing composition can be reduced greatly in aging storage of the processing compositions.
  • the solid processing composition When the moisture content exceeds 5.0 wt%, the solid processing composition will stick together in storage at high temperature.
  • the reason why the moisture content is measured is that the stability of solid processing composition at temperature is important for the following reasons, though stability in humidity is also important.
  • the temperature and humidity are not normally controlled during the transportation and an actual measured temperature of 45 - 50°C is observed. In this case, it is very difficult to control the temperature though the humidity can be controlled by moistureproofing agents or the like.
  • a solid processing composition of the invention contains at least one alkali agent and at least one of the compounds represented by the Formula [P], and when this solid processing composition is granular, it is made through granulation after the alkali agent and the compound are mixed. Even when a part of granules contains alkali agent and another part of the granules contains only a compound represented by the Formula [P], such granules are also included in the invention.
  • a tablet-form solid processing composition may be made either through compression molding after the powdery solid materials are mixed or through compression molding after the step of mixing and granulation. From the viewpoint of storage stability, a tablet-form solid processing composition made through compression molding after the step of granulation is preferable.
  • the mixture in the invention is one made through mixing or compression molding after alkali agents and paraphenylenediamine compounds are respectively granulated separately, for example, an alkali agent, paraphenylenediamine type color developing agent and preserving agent (hydroxylamine and/or its derivative) are granulated respectively and then subjected to mixing and compression molding.
  • a method for manufacturing a granular solid processing composition known methods such as rolling granulation, extrusion granulation, compression granulation, cracking granulation, stirring granulation, moving-bed granulation and spray drying granulation may be used, and from the viewpoint of granule strength of a granular processing composition, the method of stirring granulation is preferable.
  • a method for manufacturing a tablet-form solid processing composition a method employing a well-known compressor may be used.
  • a hydraulic press a single shot tablet-molding machine, a rotary tablet-molding machine and a briquetting machine may be used.
  • a tablet-form solid processing composition can take any shape, a cylindrical one is preferable from the viewpoint of productivity and ease of handling.
  • a tablet whose ratio of its diameter to its thickness is within a range of 1.0 - 6.0 is preferable and a tablet with that ratio of 2.0 - 4.0 is more preferable from the viewpoint of prevention of occurrence of powder caused by vibration during transportation.
  • the diameter of a tablet can take any value, depending on the purpose of application, its range of 5 - 50 mm is preferable and that of 7 - 30 mm is more preferable from the viewpoint of productivity.
  • the moisture content of a solid processing composition which is within a range of 0.5 - 5.0 wt% is satisfactory, but from the viewpoint of effects of the invention, the range of 0.8 - 3.5 wt% is preferable.
  • a method of granulating by the use of a solvent namely the wet type granulating method is preferable.
  • a solvent is added to raw powder materials for granulation, and the solvent used in this case includes a polar solvent such as alcohol, acetone, acetonitrile and water, or a mixture thereof. Water is preferred, as it is more explosion-proof.
  • an added amount of the above-mentioned solvent to raw materials is 1 - 10 wt%, preferably 2 - 6 wt%.
  • the added amount is less than 1 wt%, granulation can not be conducted sufficiently, while when it exceeds 10 wt%, not only may drying time be extended, but also raw materials may deteriorate in the course of granulation and drying.
  • Moisture content in the invention is a value based on all of the reduced weight, which is calculated as moisture after drying the material for one hour at 80°C by used of a commercially-available electronic moisture meter. Measurement is conducted, using a sample of about 10 g, under conditions of atmospheric pressure, temperature of 25 - 30°C and relative humidity of 40 - 45%.
  • Particle size referred to herein is a value obtained by measuring particle sizes after sieving by the use of a sieve specified in the Japanese Industrial Standards. From the viewpoint of preventing fluctuation before and after the storage, it is preferable that 60 wt% or more of particles have a particle size within the range of 149 - 1490 ⁇ m. It is more preferable that 70 wt% or more of particles have the particle size within the range of 149 - 1490 ⁇ m.
  • a 1 , A 2 and A 3 each represent a straight chained or branched alkylene group, which may be substituted and these may be either the same or different.
  • a substituent there may be given a hydroxy group, a carboxy group, a sulfonyl group, an alkoxy group, a carbamoyl group and a sulfamoyl group.
  • a 1 , A 2 and A 3 are each an unsubstituted alkylene group. More preferably A 1 , A 2 and A 3 each are -CH 2 CH 2 - or -CH(CH 3 )-CH 2 -.
  • l 1 , l 2 and l 3 each represent from 0 to 500, provided that the total number thereof is equal to or larger than 5 (l 1 + l 2 + l 3 ⁇ 5).
  • At least one of l 1 , l 2 and l 3 is 15 or more and more preferably, at least one of l 1 , l 2 and l 3 is 20 or more.
  • a block polymer (nonionic polymer of a Pluronic type) of ethylene glycol and propylene glycol represented by the following Formula [P'] is preferred.
  • Formula [P'] HO-(CH 2 CH 2 -O) l4 -[CH(CH 3 )CH 2 -O] l5 - (CH 2 CH 2 -O) l6 -H
  • l 4 , l 5 and l 6 are the same as l 1 , l 2 and l 3 defined above in the aforementioned Formula [P].
  • the content (wt%) of ethyleneoxide in the total molecular weight is 70 wt% or more, and it is especially preferred that the content is 80 wt% or more.
  • PEG polyethylene glycol
  • polyethylene glycols those having an average molecular weight ranging from 2000 to 20000 are preferred, and especially preferred includes those having an average molecular weight ranging from 3000 to 15000.
  • the average molecular weight in the invention is a molecular weight determined based on a hydroxyl value.
  • a compound represented by the aforementioned Formula [P] is contained in an amount of from 1 to 30 wt% per unit weight of solid processing composition of the invention, and from 3 to 20 wt% is more preferable. Further, compounds represented by the Formula [P] may be used independently or in combination of two or more kinds.
  • An alkali agent as used herein is a compound which shows alkalinity of pH of 8 or more in an aqueous solution thereof.
  • Preferable concrete examples include sodium carbonate, potassium carbonate, sodium bicarbonate, potassium bicarbonate, trisodium phosphate, tripotassium phosphate, , disodium phosphate, dipotassium phosphate, sodium borate, potassium borate, sodium tetraborate (borax), potassium tetraborate, sodium hydroxide, potassium hydroxide, and lithium hydroxide.
  • sodium carbonate, potassium carbonate sodium bicarbonate, sodium borate and trisodium phosphate are preferable.
  • a carbonate is especially preferable in the invention.
  • p-phenylenediamine compound in the invention those having a water-solubilizing group are used preferably because they offer the effects of the invention superbly and they cause less occurrence of fog.
  • a p-phenylenediamine compound having a water-solubilizing group not only has an advantage that a light-sensitive material is not contaminated thereby and a rash is not caused even when it sticks to the skin, but also attains efficiently an object of the invention when it is combined with a color developing solution of the invention.
  • water-solubilizing groups include the following: -(CH 2 ) n -CH 2 OH, -(CH 2 ) m -NHSO 2 -(CH 2 ) n CH 3 , -(CH 2 ) m -O-(CH 2 ) n -CH 3 , -(CH 2 CH 2 O) n C m H 2m+1 (m and n represent integers of not less than 0), -COOH group, and -SO 3 H
  • the aforementioned color developing agent is used usually in a form of a salt such as a hydrochloride, a sulfate and a p-toluenesulfonate salt.
  • R 1 and R 2 independently represent a hydrogen atom and a substituted or unsubstituted alkyl group.
  • L represents a substituted or unsubstituted, straight-chained or branched alkylene group having from 1 to 10 carbons, preferably from 1 to 5.
  • methylene, ethylene, trimethylene and propylene are given, and as a substituent, a carboxyl group, a sulphone group, a phosphone group, a phosphinic acid agroup, a hydroxy group, a cyano group and an ammonio group which may be substituted by an alkyl group having from 1 to 5 carbon atoms are given.
  • A represents a carboxyl group, a sulfone group, a phosphone group, a phosphinic acid residue, a hydroxy group, a cyano group, an alkoxy group, an amino group which may have an alkyl group having 1 to 5 carbon atoms, an ammonio group which may have an alkyl group having 1 to 5 carbon atoms, a carbamoyl group which may have an alkyl group having 1 to 5 carbon atoms, a sulfamoyl group which may have an alkyl group having 1 to 5 carbon atoms and a substituted or unsubstituted alkylsulfonyl group.
  • A-L- examples include carboxymethyl, carboxyethyl, carboxypropyl, sulfoethyl, sulfopropyl, sulfobutyl, phosphonomethyl, phosphonoethyl, methoxyethyl, cyanoethyl and hydroxyethyl.
  • R 3 represents a hydrogen atom, a substituted or unsubstituted, straight-chained or branched alkyl group having from 1 to 10 carbon atoms.
  • the substituent includes a carboxyl group, a sulfo group, a phosphone group, a phosphonic acid residue, a hydroxy group, a cyano group, an alkoxy group, a carbamoyl group and an ammonio group which may have an alkyl group having 1 to about 5 carbon atoms, provided that L and R may combine to form a ring.
  • These compounds are used as an isolated amine and also as a salt such as a hydrochloride, a sulfate, an oxalate, a p-toluenesulfonate, an alkali metal salt and an ammonium salt.
  • a salt such as a hydrochloride, a sulfate, an oxalate, a p-toluenesulfonate, an alkali metal salt and an ammonium salt.
  • R 1 R 2 A-1 -H -H A-2 -H -CH 3 A-3 -CH 3 -CH 3 A-4 -H -C 2 H 5 A-5 -CH 3 -C 2 H 5 A-6 -C 2 H 5 -C 2 H 5 A-7 -C 3 H 7 (n) -C 3 H 7 (n) A-8 -C 3 H 7 (i) -C 3 H 7 (i) A-9 -C 4 H 9 (n) -C 4 H 9 (n) A-10 -C 4 H 9 (i) -C 4 H 9 (i) A-11 -C 4 H 9 (t) -C 4 H 9 (t) A-12 -CH 3 -CH 2 CH 2 COOH A-13 -CH 3 -CH 2 CH 2 SO 3 H A-14 -CH 3 -CH 2 COOH A-15 -CH 3 -CH 2 CH 2 PO 3 H 2 A-16
  • a sulfite, a bisulfite or a metabisulfite is added to the solid processing composition of the invention.
  • Specific examples of the aforementioned sulfite, bisulfite, metabisulfite include sodium sulfite, potassium sulfite, sodium bisulfite, potassium bisulfite, sodium metabisulfite and potassium metabisulfite.
  • Preferable one includes sodium sulfite and potassium sulfite, and these compounds can be used in an arbitrary form of an anhydrous salt and hydrous salt. In the case of the hydrous salt, however, the one wherein water is not isolated at 50°C or less is especially preferable in terms of the effects of the invention.
  • a halide there may be given potassium chloride, sodium chloride, potassium bromide, sodium bromide, potassium iodide and sodium iodide.
  • the solid processing composition of the invention may contain a chelating agent represented by the following Formula [I].
  • T 1 represents a hydrogen atom, a hydroxy group, a carboxy group, a sulfo group, a carbamoyl group, a phosphono group, a phosphone group, a sulfamoyl group, a substituted or unsubstituted alkyl group, an alkoxy group, an alkylsulfonamide group, an alkylthio group, an acylamino group, a hydroxamic acid group, a hydroxyalkyl group or W 1 represents a substituted or unsubstituted alkylene group, an arylene group, an alkenyl group, a cycloalkylene group, an aralkylene group or X represents -O-, -S-, a divalent heterocycle or R 11 through R 15 independently represent a hydrogen atom, a hydroxy group, a carboxy group, a sulfo group, a carbamoyl group, a phospho
  • Exemplified compounds of the aforesaid chelating agent that improves the effects of the invention include (I-1) to (I-8), (I-12), (I-14) to (I-20), (I-22), (I-23) and (I-27). Among those, more preferred are (I-1), (I-2), (I-3), (I-5), (I-6), (I-12), (I-14), (I-15) or (I-17). These compounds can be used in a form of a free acid, sodium salt and potassium salt. Especially preferred is the sodium salt.
  • the saccharides in the invention refer to monosaccharides or polysaccharides in which monosaccharides are combined with each other through a glycosid bond including a derivative thereof or a decomposition product thereof.
  • Monosaccharides referred to herein include a polyhydroxy aldehyde, polyhydroxy ketone and their derivatives such as reduction derivatives, oxidation derivatives, deoxy-derivatives, aminoderivatives or thio-derivatives. Most of them are represented by the general formula C n' (H 2 O)m'.
  • the monosaccharide used in the invention includes a compound derived from the saccharide skeleton represented by the above formula.
  • Preferred is a sugar alcohol having a primary or secondary alcohol group to which an aldehyde or ketone group is reduced.
  • Polysaccharides include celluloses, starches or glycogens.
  • the celluloses include derivatives such as cellulose ethers in which all or a part of the hydroxy groups are etherified, and starches include various hydrolysis and decomposition compounds thereof, such as maltose or dextrins.
  • Celluloses may be in an alkali salt form in view of solubility.
  • Preferred polysaccharides are celluloses or dextrins, and dextrins are more preferably used.
  • B-(66) to (83) are preferably used, and B-(69) and B-(74) to (83) are more preferably used.
  • C-(21) to (55) are preferably used, and compounds, C-(36) to (55) are more preferably used.
  • the weight average molecular weight of dextrins used in the composition of the invention may be any, but it is preferably 10 to 10000.
  • Starch compounds available on the market include Pineflow, Pine-dex series, Max 100, Glistar P, TK-16, MPD, H-PDX and Stuco-dex produced by Matsutani Kagaku Co., Ltd. or Oil Q series produced by Nihon Yushi Co., Ltd.
  • Alkali agent (Compound described on Table 1) 13000 g Compound represented by Formula [P], as described in Table 1 2000 g
  • the granules thus obtained were dried by a commercially-available moving-bed dryer, while controlling the temperature of hot air to be at 50 - 65°C in the course of drying.
  • the granules were subjected to grain-dressing by a commercially-available granulating machine, with the use of a 1.5 mm-mesh screen.
  • the granular samples (1-1) to (1-26) thus prepared were vibrated for one minute by a micro-type electromagnetic vibration screening machine (Model M-100) by the use of a screen with 100 ⁇ m-mesh. After fine powder is removed completely, samples weighing 50 g on the screen were put in an opened laboratory dish to prepare two of each of the various samples, which were stored for three hours in the environmental chamber where the temperature was 25°C and relative humidity was 45%. After the storage, the granular samples were screened again by the screen with 100 ⁇ m-mesh under the above-mentioned conditions, to test the occurrence of powder after storage.
  • a micro-type electromagnetic vibration screening machine Model M-100
  • Example 2 Each of the above-mentioned compounds was crushed and granulated in the same manner as in Example 1. In this case, the amount of water added was 4 wt% of the total weight used for granulation, and granules thus obtained were dried until the moisture content was from 1.5 to 2.0 wt%.
  • Example 2 The resulting granules were subjected to grain-dressing in a similar manner to Example 1.
  • the samples thus obtained were defined to be granular samples (2-1) to (2-11).
  • Granular samples (2-12) - (2-22) were prepared from the above-mentioned compounds through the same manner as in Operation (2-1).
  • Granule (A) The above-mentioned granules were subjected to grain size-dressing by a grain size-selecting machine, and classified by the use of a screen to control them within a range of particle size from 149 to 1490 ⁇ m. This was defined to be Granule (A).
  • the above compounds were crushed by a commercially-available hammer mill to a particle size of 149 ⁇ m or less.
  • crushed compounds were mixed sufficiently by a commercially-available stirring and granulating machine, and then water was added thereto for granulation.
  • An amount of water added in this case was 3 wt% of the total weight of the crushed compounds.
  • These granules were dried by a commercially-available moving-bed dryer until the moisture content (at 80°C) was from 1.5 to 2.0 wt% while controlling the temperature of hot air for drying at from 50 to 60°C.
  • the granules were size-selected by a commercially-available grain size-dressing machine during the course of drying and after drying, and then classified by the use of a screen to control the particle size of the granules within a range of from 149 to 1490 ⁇ m.
  • the aforementioned granular samples after being stored were mixed again by the mixing machine.
  • the samples after mixing each weighing 10 g were picked up 10 times to test for fluctuation of solid processing composition through determination of the paraphenylenediamine compound.
  • Table 3 shows the results of the evaluation.
  • Granular samples were prepared in the same manner as in Example 1.
  • sodium myristoyl-N-methyl- ⁇ -alanine crushed to a particle size of 100 ⁇ m or less was added in an amount of 0.5 wt% of the total weight of the solid processing composition, and then they were mixed for 3 minutes by a commercially-available cross-rotary mixing machine.
  • the mixed granules were subjected to continuous tablet-molding on the modified rotary tableting machine, Clean Pressed Correct 18K made by Kikusui Manufacturing Co., Ltd. Tablets were prepared under conditions that a diameter of a tablet was 15 mm, weight of a tablet was 1.5 g and pressure for compression was 1400 kg/cm 2 (Samples 4-1 to 4-26).
  • Alkali agent (compound described on Table 5) 13000 g
  • the compounds were each crushed to a particle size of 149 ⁇ m or less by a commercially-available hammer mill. These crushed compounds were granulated in a commercially-available stirring and granulating machine by adding water thereto.
  • the granules thus obtained were dried by a commercially-available moving-bed drying machine while controlling the temperature of hot air for drying to be at from 50 to 65°C.
  • the granules were size-selected by a commercially-available size-selecting machine by the use of a 1.5 mm screen during the course of drying and after drying. Further, the amount of water added for granulation and the drying time were adjusted appropriately so that the moisture content shown on Table 5 was obtained.
  • tablet-shaped Sample (4-1) to (4-37) were prepared.
  • the tablet-shaped samples thus prepared were put in an open laboratory dish so that two each for respective samples were prepared. They were stored for 3 hours in an environmental chamber where temperature and relative humidity were maintained at 25°C and 45% respectively. Each sample after storage was vibrated for 1 minute by a micro-type electromagnetic vibrator (Model M-100) with a screen with 100 ⁇ m-mesh, and occurrence of fine powder after storage was tested.
  • Model M-100 micro-type electromagnetic vibrator
  • Tables 4 and 5 show the results of the evaluation.
  • an alkali agent is a carbonate and a compound represented by Formula [P] is polyethyleneglycol having an average molecular weight of from 2000 to 20000, more effects of the invention are exhibited.
  • the moisture content that is within 0.5 to 5.0 wt% is satisfactory, but when it is within 0.8 to 3.5 wt%, more effects of the invention can be exhibited.
  • Granular samples were prepared in the same manner as in Example 2.
  • tablet-form Samples (5-1) to (5-22) were prepared in the same manner as in Example 4.
  • Samples were prepared under the condition that the diameter of a tablet was 20 mm, the weight of a tablet was 2.6 g and the pressure for compression was 1400 kg/cm 2 .
  • polyethyleneglycol is added in an amount of from 1.0 to 30 wt% per unit weight, preferably form 3.0 to 20.0 wt%.
  • Granules (A), (C) and (E) were prepared in the same manner as in Example 3.
  • Granules (A), (C) and (E) were mixed for 10 minutes by a commercially-available cross-rotary mixing machine, then sodium myristoyl-N-metyl- ⁇ -alanine was added thereto in an amount of 0.5 wt% of the total weight of the mixture to be mixed for another 3 minutes, and thereby tablet-form samples (6-1) to (6-6) were prepared in the same manner as in Example 4.
  • the diameter of a tablet was 30 mm
  • the weight of a tablet was 12.0 g
  • the pressure for compression was 1400 kg/cm 2 .
  • Granules (B), (D) and (F) were subjected to mixing and compression-molding under the same conditions for preparation as in Operation (6-1), and thereby tablet-shaped samples (6-7) to (6-12) were prepared.

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

Claims (9)

  1. Körnige feste Behandlungszusammensetzung, die zur Verwendung bei der Herstellung einer Farbentwicklerlösung für ein farbphotographisches Silberhalogenidaufzeichnungsmaterial geeignet ist, wobei die feste Behandlungszusammensetzung ein alkalisches Mittel, das in einer wässrigen Lösung eine Alkalinität des pH-Werts 8 oder mehr zeigt, und eine Verbindung der im folgenden angegebenen Formel [P] umfasst und einen Feuchtigkeitsgehalt von 0,5-5 Gew.-% aufweist, wobei der Feuchtigkeitsgehalt ein auf der gesamten Gewichtsverminderung der Zusammensetzung nach dem Trocknen der Zusammensetzung während 1 h bei 80 °C beruhender Wert ist: Formel [P]   HO-(A1-O)l1-(A2-O)l2-(A3-O)l3-H worin A1, A2 und A3 unabhängig voneinander für eine optional substituierte, geradkettige oder verzweigtkettige Alkylengruppe stehen; l1, l2 und l3 unabhängig voneinander 0 bis 500 sind und die Summe von l1, l2 und l3 mindestens 5 beträgt,
    unter dem Vorbehalt, dass eine körnige feste Behandlungszusammensetzung, die durch Vermischen von Natrium-p-toluolsulfonat, Toluolsulfit, Kaliumhydroxid, Polyethylenglykol (mittleres Molekulargewicht 6000), Kaliumcarbonat und D-Mannit unter Zugabe von Wasser und Trocknen des erhaltenen Granulats bei 40 °C während 12 h, um den Feuchtigkeitsgehalt auf 1 % oder weniger zu reduzieren, hergestellt ist, ausgeschlossen ist.
  2. Körnige feste Behandlungszusammensetzung gemäß Anspruch 1, worin das alkalische Mittel ein Carbonat ist.
  3. Körnige feste Behandlungszusammensetzung gemäß den Ansprüchen 1 oder 2, worin die Verbindung der Formel [P] in einer Menge von 1,0-30,0 Gew.-% vorliegt.
  4. Körnige feste Behandlungszusammensetzung gemäß Anspruch 3, worin die Verbindung der Formel [P] Polyethylenglykol ist.
  5. Körnige feste Behandlungszusammensetzung gemäß Anspruch 4, worin das Polyethylenglykol ein mittleres Molekulargewicht von 2000-20000 aufweist.
  6. Körnige feste Behandlungszusammensetzung gemäß einem der vorhergehenden Ansprüche, wobei die feste Behandlungszusammensetzung mit einer granulierten p-Phenylendiaminverbindung unter Bildung eines Gemischs vermischt ist.
  7. Körnige feste Behandlungszusammensetzung gemäß einem der vorhergehenden Ansprüche, worin mindestens 60 Gew.-% der festen Behandlungszusammensetzung eine Teilchengröße von 149-1490 µm aufweisen.
  8. Verfahren zur Herstellung einer festen Behandlungszusammensetzung in Form einer Tablette mit einem Feuchtigkeitsgehalt von 0,5-5 Gew.-%, wobei dieses Verfahren das Formpressen einer körnigen festen Behandlungszusammensetzung gemäß einem der Ansprüche 1 bis 7 unter Bildung einer Tablette umfasst.
  9. Verfahren zur Herstellung einer festen Behandlungszusammensetzung in Form einer Tablette mit einem Feuchtigkeitsgehalt von 0,5-5 Gew.-%, wobei dieses Verfahren das Vermischen einer granulierten p-Phenylendiaminverbindung mit einer körnigen festen Behandlungszusammensetzung gemäß einem der Ansprüche 1 bis 7 zur Bildung eines Gemischs und das Formpressen des Gemischs zur Herstellung der Tablette umfasst.
EP95303857A 1994-06-10 1995-06-06 Farbentwicklungszusammensetzung in Granulat- oder Tablettenform Expired - Lifetime EP0687951B1 (de)

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JP12915794 1994-06-10
JP129157/94 1994-06-10
JP12915794 1994-06-10

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EP0687951A1 EP0687951A1 (de) 1995-12-20
EP0687951B1 true EP0687951B1 (de) 2001-10-10

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