JP2003015242A - Method and device for dissolving gel-like object for photographic material - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a method and a device for dissolving a gel-like object for photographic material whose dissolving property is improved so that a prescribed flow rate can be secured not only at regular time but also at the time when residual amount in a tank is reduced at the termination of manufacture by using a tank-like dissolving device in the dissolution of the gel-like object used as the photographic material. SOLUTION: In the dissolving method, the gel-like object is dissolved by heating it by a jacket in a dissolving tank or by simultaneously promoting heat transmission with a stirring means. A means for detecting a temperature is arranged at the exit of the dissolving tank or just behind the dissolving tank. A means measuring dissolving speed is disposed in a process for using the dissolved gel-like object or in the middle of the piping. The heat insulating temperature of the dissolving tank jacket is controlled in accordance with the flow-rate signal of the flowing dissolved gel-like object and/or a temperature signal.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method and an apparatus for preparing a gel-like material for a photographic light-sensitive material, and more particularly to the construction of a production system corresponding to an increase in the number of varieties of photographic light-sensitive materials. As a part, the present invention relates to a method for dissolving a raw material used for producing a silver halide photographic light-sensitive material, which has a property of forming a gel at a low temperature and a sol at a high temperature.

[0002]

2. Description of the Related Art The manufacture of photographic light-sensitive materials has a long history,
The emulsions and emulsions used in this production are generally stored after they are produced under low temperature conditions, their quality is checked, and after confirming that there is no problem, they are applied to a support to produce products. Emulsions and emulsions are stored as protective colloid solutions such as gelatin and agar. Such a protective colloid has a property of forming a gel at a low temperature and a sol at a high temperature, and at the time of actual coating, emulsions and emulsions stored in a gel state must be dissolved to prepare a coating solution. . Therefore, the dissolution of emulsions and emulsions is one of the important steps in the production of photographic light-sensitive materials, and the photographic light-sensitive material manufacturers have applied for a number of patents on the dissolution. Japanese Patent Publication Sho 44-9
Japanese Patent Publication No. 495 and Japanese Patent Publication No. 51-1738 disclose a pot-type melting device. This method is a method in which a solution is stored in a pot and has a heat transfer surface in the gel-like pot, and the dissolving device is pressed against its own weight or mechanically, and the dissolved liquid is drawn out by means such as a pump. This method is not a problem when the production amount is small, but when the coating speed increases and a higher dissolution rate is required, it is necessary to install multiple similar devices and the pots are empty. When this happens, it is necessary to change the pot to the next pot, which is not suitable for mass production and multi-product production. In Japanese Utility Model Publication No. 49-34816, a method of continuous-type melting instead of batch-type melting, which is a drawback of the pot-melting method, was developed. This system was developed with the aim of quickly transferring heat from the heat transfer surface to the gel-like substance and melting it, and various innovations have been made such as rotating the heat transfer surface. However, since the structure has a dynamic part, the structure is complicated, the cost is high, and the maintenance is difficult. JP-A-55
In the method of Japanese Patent No. 159928, in order to increase the heat transfer efficiency, the melting capacity is increased by rotating the heat transfer surface of the pipe structure, but it has the same problem.

Further, Japanese Examined Patent Publication No. 50-31447 discloses a static melting device in which the heat transfer surface is formed by a pipe having a slatted shape. This method addresses the problems of the dynamic method such as cost and maintenance, but conversely,
It is indispensable to use it in a special or near-dedicated state, and it lacks adaptability as a facility in the small-quantity, high-mix age. JP-A-57
No. 169743 discloses a pot melting method using microwaves. In addition, Japanese Patent Laid-Open No. 14542/1989
A similar system is also proposed in Japanese Patent Publication No. 8. Japanese Patent Laid-Open No. 61-73945 also discloses a method using microwaves. However, handling microwaves on an industrial scale and arranging a large number of microwaves is extremely difficult due to electromagnetic wave problems and equipment cost problems. In addition, the electromagnetic waves tend to concentrate on the liquid and are consumed more when the temperature of the dissolved liquid is raised rather than when the dissolving ability is raised, which is inefficient.

In Japanese Patent Publication No. 3-16008, a gel-like substance is finely crushed by a mechanical force and heat is exchanged thereafter, so that the heat transfer efficiency is very good and high-performance melting is possible, but it is dynamic. Since a crusher and a feeder are required as means, there is a drawback that the apparatus cost becomes high. JP 63
Japanese Patent Laid-Open No. -100439 discloses a stirring method for increasing heat transfer efficiency and a method for promoting separation of a dissolved liquid and a gel-like material in order to dissolve a necessary amount when needed in a dissolution method using a tank-type dissolution device. A method for controlling dissolution to a higher degree has been disclosed, such as combination, detecting the amount of dissolution, and controlling dissolution by stirring. Further, in Japanese Patent Laid-Open No. 9-85069, for the purpose of improving heat transfer by a stirring method and reducing the cost, the gel-like substance in the dissolution tank is finely crushed by blades of a stirrer and a baffle plate attached to the dissolution tank, And, a method of heating and melting the gelled substance by giving a solid flow to the whole gelled substance in the dissolution tank has been disclosed. By adopting such a method, the dissolution capacity could be dramatically improved. At steady state, the capacity is very high, especially when a certain amount of gel is present in the tank, but as the remaining amount in the tank decreases as the production is approached, the dissolution capacity decreases and the supply capacity becomes insufficient. There is a drawback to

[0005]

SUMMARY OF THE INVENTION Accordingly, an object of the present invention is to provide a method and apparatus for dissolving a gel-like material for a photographic light-sensitive material, and more particularly a method and apparatus for dissolving a gel-like material, which overcomes the above problems. That is. That is, using a tank-type dissolving device, a method for dissolving a gel-like substance for a photographic light-sensitive material, which has improved solubility so that a predetermined flow rate can be obtained not only in a steady state but also when the remaining amount in the tank is reduced at the end of production And to provide a device.

[0006]

As a result of intensive studies by the present inventors, the above object of the present invention can be achieved by the following method and apparatus. That is, the present invention is as follows. (1) In the dissolution method, a gel material used as a photographic light-sensitive material is heated by a jacket in a dissolution tank, or heated by a jacket in a dissolution tank and accelerated by heat transfer by a stirring means to be dissolved. A means for detecting the temperature is arranged at the tank outlet or immediately after the dissolution tank, and a step for using the melted gel-like material, or a means for measuring the dissolution rate in the middle of the pipe is arranged, and the melted gel-like material flows. According to the flow rate signal and / or the temperature signal,
A method for dissolving a gel-like material for a photographic light-sensitive material, which comprises adjusting and controlling a heat retention temperature of a dissolution tank jacket. (2) In the method for dissolving a gel-like material for a photographic light-sensitive material as described in (1) above, the photographic performance and physical properties (viscosity, pH, conductivity, etc.) of the gel-like substance are measured and evaluated in advance,
The temperature of the heat medium supplied to the jacket of the dissolution tank is adjusted so that the temperature of the eluting gel-like substance becomes the specified temperature, with the upper limit of the temperature that does not cause adverse effects due to the high temperature of the eluting gel-like substance. Then, the method for dissolving a gel-like substance for a photographic light-sensitive material is characterized in that it is dissolved while controlling the heat retention temperature. (3) In the method for dissolving a gel-like material for a photographic light-sensitive material as described in (1) or (2) above, if the dissolution rate measurement result is faster than the dissolution rate required from the next step, the dissolution temperature is set to A method for dissolving a gel-like substance for a photographic light-sensitive material, which comprises controlling the temperature to decrease and controlling the temperature to increase when the dissolution rate is insufficient.

(4) In the method of dissolving a gel-like material for a photographic light-sensitive material as described in (3) above, controlling the temperature of the heat medium supplied to the jacket of the dissolution tank when the dissolution rate is insufficient, and / Alternatively, a method for dissolving a gelled material for a photographic light-sensitive material, characterized in that the supply rate of a heat medium required for the jacket is controlled independently of the temperature. (5) In a melting device for melting a gel-like material used as a photographic light-sensitive material, comprising a jacket or a dissolution tank equipped with a jacket and a stirring means, the temperature is detected immediately after the dissolution tank outlet or immediately after the dissolution tank. And a means for measuring the dissolution rate in the process of using the dissolved gel-like material, or in the middle of the piping, according to the flow signal of the melted gel-like material and / or the temperature signal. A device for dissolving a gel-like substance for a photographic light-sensitive material, characterized in that means for adjusting and controlling the heat retention temperature of the jacket is arranged.

A method and an apparatus for dissolving a gel-like substance for a photographic light-sensitive material of the present invention is a method for dissolving a gel-like substance used as a photographic light-sensitive material. By controlling the jacket temperature, it is possible to dissolve at a constant rate, and the changes in photographic performance and physical properties (viscosity, pH, electric conductivity, etc.) of the dissolved liquid can be made constant. Very effective merits were obtained in terms of practical use, such as the fact that it became possible to dissolve at a constant rate even when the amount of a certain gel-like material became small.

[0009]

BEST MODE FOR CARRYING OUT THE INVENTION The method and apparatus for dissolving a gelled material for a photographic light-sensitive material of the present invention will be described in detail below. JP-A-9-85069 or JP-A-63-10.
As disclosed in Japanese Patent No. 0439, in a dissolution method using a tank having a stirrer in the tank and a heat insulation jacket, a means for measuring the temperature of the eluate of the gel substance is provided at the outlet of the dissolution device, This is a dissolution method characterized by controlling the temperature of the liquid supplied to the tank jacket so that the temperature of the eluate does not rise above a specified temperature, according to the capacity information and the signal of the temperature of the liquid to elute. It is also applicable to. The predetermined temperature is the upper limit temperature in a range in which the temperature dependence of the viscosity of the gel-like substance is measured and evaluated in advance and no adverse effect is caused due to the high temperature of the gel-like substance to be eluted.

For example, when gelatin is used as a protective colloid which forms a gel-like substance, the sol-gel conversion temperature is 25 to 30 although the concentration used varies slightly.
It is about ℃. In the case of heat transfer melting, the main factor that influences the ability is the temperature difference between the heat source and the melt, and it is common sense that increasing this temperature will increase the melting rate. However, as already introduced, each of the sensitive material makers has a long history, but it is negative to raise the melting temperature, and some of these problems are described in some patents. ing. In fact, the same tendency can be confirmed by examining some gel substances targeted by the present invention. However, observing such a phenomenon in detail, the sol-
The viscosity of the gel-like substance at the temperature of gel conversion has a viscosity of more than 1000 cp even when measured by a C-type viscometer, and is not a practical viscosity. The temperature at which the actually dissolved liquid is used is at least 5 ° C, preferably at least 10 ° C, higher than the sol-gel conversion temperature. Therefore, the gel-like substance eluted from the dissolution apparatus is usually designed to be stable up to such a temperature, and considering various manufacturing conditions, even if the temperature is higher than this temperature by 2 to 3 ° C. It is considered not to be. It was also found that when the dissolution temperature was raised, the liquid temperature of the eluate also increased, the viscosity of the gel substance liquid decreased, and the discharge speed increased, resulting in that the temperature was not as high as expected.
Therefore, it was found that the dissolution capacity can be improved by paying attention to the temperature of the liquid to be eluted as a means for increasing the heat transfer efficiency and controlling the temperature so as not to exceed a predetermined temperature. Based on such experimental facts, when the dissolution rate is sufficient, the dissolution temperature is lowered, or the heat source supplied to the jacket is stopped, or the heat source at a temperature not higher than the gelation point of the gel substance in the jacket. By controlling the melting rate by supplying and cooling, the melting rate is controlled by controlling the temperature and flow rate of the heat source supplied to the jacket so that the elution temperature does not reach the specified temperature when the melting capacity is insufficient. Is a dissolution method.

An embodiment of the present invention will be described with reference to the drawings.
FIG. 1 is a schematic view showing an apparatus 1 to which the method for dissolving a gel-like material for a photographic light-sensitive material according to the present invention is applied. The dissolution tank 2 is a system having a heat insulation jacket 7 and a stirring device 8 similar to the system described in JP-A-63-100439 or JP-A-9-85069, or a jacket 7 without the stirring device 8. A melting tank 2 equipped only with a temperature control device 3 (generally referred to as a constant temperature tank or heat transfer system) for supplying a temperature-controllable heat source to the jacket 7. 2 bottom, or
The temperature sensor 4 is provided in the pipe 9 immediately after the dissolution tank 2, and a means 6 (generally, various flowmeters) for measuring the dissolution rate in the step of using the solution of the dissolved gel-like substance or on the way up to that step. Alternatively, a balance for measuring the weight per unit time, or a tod cell, etc. is provided, and static mixing is performed to bring the temperature to the next step or the temperature required for the next step before the dissolution rate measuring means 6. And a heat exchange means 5 having a dynamic mixer, a temperature sensor 4 and a dissolution rate measuring means 6
A gel-like material used as a photographic light-sensitive material that has a dissolution control device that captures the signal of a sensor such as, and controls the dissolution by controlling the amount of solution supplied to the dissolution tank jacket and the temperature of the solution according to this control. The melting device 1.

Various chemicals to be dissolved and prepared by using the method and apparatus for preparing a chemical solution of a gel-like material for a photographic light-sensitive material of the present invention,
The photographic light-sensitive material will be described. The photographic light-sensitive material may have at least one light-sensitive layer provided on the support. As a typical example, a silver halide photographic light-sensitive material having on a support at least one light-sensitive layer composed of a plurality of silver halide emulsion layers having substantially the same color sensitivity but different sensitivities. Is. The photosensitive layer is a unit photosensitive layer having color sensitivity to any of blue light, green light, and red light, and in a multilayer silver halide color photographic light-sensitive material, the arrangement of the unit photosensitive layers is generally The red color-sensitive layer, the green color-sensitive layer and the blue color-sensitive layer are arranged in this order from the support side.
However, the order of installation may be reversed depending on the purpose, or the order of installation may be such that different photosensitive layers are sandwiched between the same color-sensitive layers. A non-photosensitive layer may be provided between the above-described silver halide photosensitive layers and as the uppermost layer and the lowermost layer. These may contain a coupler, a DIR compound, a color mixing inhibitor, etc. described later. A plurality of silver halide emulsion layers constituting each unit photosensitive layer is DE 1,121,470 or GB 92
As described in 3,045, it is preferable to arrange two layers of a high-sensitivity emulsion layer and a low-sensitivity emulsion layer so that the photosensitivity becomes lower toward the support. Further, JP-A-57-112751, JP-A-62-200350, JP-A-62-206541 and JP-A-6-2003541.
As described in JP-A-2-206543, a low-sensitivity emulsion layer may be provided on the side farther from the support and a high-sensitivity emulsion layer may be provided on the side closer to the support.

As a specific example, from the side farthest from the support,
Low sensitivity blue photosensitive layer (BL) / High sensitivity blue photosensitive layer (BH) / High sensitivity green photosensitive layer (GH) / Low sensitivity green photosensitive layer (GL) / High sensitivity red photosensitive layer (RH) / Low sensitivity red photosensitive layer (RL) order, or BH / BL / GL / GH / RH / RL order, or BH / BL / GH /
It can be installed in the order of GL / RL / RH. In addition,
As described in JP-A-55-34932, the blue-sensitive layer / GH / RH / GL / RL may be arranged in this order from the side farthest from the support. Also, JP-A-56-25738 and 62-6
As described in Japanese Patent No. 3936, the blue-sensitive layer / GL / RL / GH / RH may be arranged in this order from the side farthest from the support. Further, as described in JP-B-49-15495, the upper layer is a silver halide emulsion layer having the highest sensitivity,
The middle layer is a silver halide emulsion layer having a lower photosensitivity, and the lower layer is a silver halide emulsion layer having a lower photosensitivity than the middle layer. The photosensitivity is gradually reduced toward the support. An arrangement composed of three layers can be mentioned. Even when it is composed of three layers having different sensitivities, as described in JP-A-59-202464, a medium-sensitivity emulsion layer from the side distant from the support in the same color-sensitive layer. / High-speed emulsion layer / low-speed emulsion layer may be arranged in this order. In addition, the layers may be arranged in the order of high-speed emulsion layer / low-speed emulsion layer / medium-speed emulsion layer, or low-speed emulsion layer / medium-speed emulsion layer / high-speed emulsion layer. Also, in the case of four or more layers, the arrangement may be changed as described above. USP 4,663,271, USP 4,705,744, USP 4,707,43 to improve color reproducibility
6, mainly using a donor layer (CL) having a multi-layer effect having a spectral sensitivity distribution different from that of the main photosensitive layers such as BL, GL, and RL described in JP-A-62-160448 and 63-89850. It is preferably arranged adjacent to or in proximity to the photosensitive layer.

The preferred silver halide used in the photographic light-sensitive material is silver iodobromide, silver iodochloride, or silver iodochlorobromide containing about 30 mol% or less of silver iodide. Particularly preferred is silver iodobromide or silver iodochlorobromide containing from about 2 mol% to about 10 mol% silver iodide. The silver halide grains in a photographic emulsion are those having regular crystals such as cubes, octahedra and tetradecahedrons, those having irregular crystal shapes such as spheres and plates, twin planes, etc. It may have a crystal defect of, or a composite form thereof. The grain size of silver halide may be fine grains of about 0.2 μm or less or large grains having a projected area diameter of up to about 10 μm, and may be a polydisperse emulsion or a monodisperse emulsion. The silver halide photographic emulsion is, for example, Research Disclosure (hereinafter, R
No.17643 (December 1978), pp. 22-23, "I.
Emulsion preparation and types ", and No. 18716 (November, 1979), 648, No. 307105 (19).
1989, 863-865, and Graphide, Physics and Chemistry of Photography, published by Paul Montel (P.Glafkides, Chi.
mie et Phisique Photographiques, Paul Montel, 196
7), "Photoemulsion Chemistry" by Duffin, published by Focal Press (GF Duffin, Photographic Emulsion Chemistr
y, Focal Press, 1966), "Production and Coating of Photographic Emulsions" by Zelikmann et al., published by Focal Press (VL Zelikman,
et al., Making and Coating Photographic Emulsion, F
Ocal Press, 1964) and the like. The monodisperse emulsions described in USP 3,574,628, 3,655,394 and GB 1,413,748 are also preferable. Further, tabular grains having an aspect ratio of about 3 or more can be used in the present invention. Tabular grains are described in Gutoff, Photographic Science and Engineering,
Volume 14, Pages 248-257 (1970); US 4,434,226, 4,41.
4,310, 4,433,048, 4,439,520 and GB 2,112,15
It can be easily prepared by the method described in 7. The crystal structure may be uniform, may have different halogen compositions inside and outside, or may have a layered structure. Silver halides having different compositions may be joined by epitaxial joining, and may be joined with a compound other than silver halide such as silver rhodanide and lead oxide. Also, a mixture of particles having various crystal forms may be used.

The above-mentioned emulsion may be either a surface latent image type which forms a latent image mainly on the surface, an internal latent image type which is formed inside the grain or a type which has a latent image on both the surface and the inside. Must be a type of emulsion. Among the internal latent image type emulsions, core / shell type internal latent image type emulsions described in JP-A-63-264740 may be used, and the preparation method thereof is described in JP-A-59-133542. . The thickness of the shell of this emulsion varies depending on the development process etc., but is 3-40 nm.
Is preferable, and 5 to 20 nm is particularly preferable. As the silver halide emulsion, those which are physically ripened, chemically ripened and spectrally sensitized are usually used. Additives used in such a process are described in RD No. 17643, RD No. 18716 and RD No. 307105, and the corresponding portions are summarized in the table below. For the light-sensitive material, two or more kinds of emulsions having different characteristics of at least one of the grain size, grain size distribution, halogen composition, grain shape, and sensitivity of the photosensitive silver halide emulsion are mixed and used in the same layer. be able to. US Pat. No. 4,082,553, the surface of which is covered with silver halide grains, US Pat.
98, JP-A-59-214852, wherein the internally fogged silver halide grains and colloidal silver are applied to a photosensitive silver halide emulsion layer and / or a substantially non-photosensitive hydrophilic colloid layer. Preferably. The fogged silver halide grain inside or on the surface means a silver halide grain which enables uniform (non-imagewise) development regardless of the unexposed area and exposed area of the light-sensitive material. , Its preparation method is described in US Pat. No. 4,626,498 and JP-A-59-214852. The silver halide forming the inner core of a core / shell type silver halide grain having a fogged inside may have a different halogen composition. As the silver halide whose inside or surface is fogged, any of silver chloride, silver chlorobromide, silver iodobromide and silver chloroiodobromide can be used.
The average grain size of these fogged silver halide grains is preferably 0.01 to 0.75 .mu.m, more preferably 0.05 to 0.6 .mu.m. The grain shape may be regular grain or polydisperse emulsion, but monodispersity (at least 95% of the weight or number of silver halide grains has a grain size within ± 40% of the average grain size). It is preferable that

It is also preferable to use non-photosensitive fine grain silver halide. The non-photosensitive fine grain silver halide is a fine grain of silver halide which is not exposed to light during imagewise exposure for obtaining a dye image and is not substantially developed in the development process, and it is preferable that it is not fogged in advance. . The fine grain silver halide has a silver bromide content of 0 to 100 mol%, and may optionally contain silver chloride and / or silver iodide. Preferably silver iodide
0.5 to 10 mol% is contained. Fine grain silver halide has an average grain size (average value of circle equivalent diameter of projected area) of 0.
01 to 0.5 μm is preferable, and 0.02 to 0.2 μm is more preferable. The fine grain silver halide can be prepared by a method similar to that for ordinary photosensitive silver halide. The surface of the silver halide grain does not need to be optically sensitized nor spectrally sensitized. However, prior to adding this to the coating liquid, it is preferable to add a known stabilizer such as a triazole-based, azaindene-based, benzothiazolium-based, mercapto-based compound or zinc compound in advance. Colloidal silver can be contained in the fine silver halide grain-containing layer. Coated silver amount of the light-sensitive material of the present invention is preferably 6.0 g / m ² or less, 4.5 g / m ² or less is most preferred.

Photographic additives are also listed in the RD and the relevant locations are indicated in the table below.

[0018] (Types of additives) (RD17643) (RD18716) (RD307105) 1. Chemical sensitizer page 23 page 648 page right column page 866 2. Sensitivity enhancer page 648, right column 3. Spectral sensitizer, pages 23 to 24, page 648, right column, pages 866 to 868     Supersensitizer ~ 649, right column 4. Whitening agent page 24 page 647 page right column page 868 5. Light absorber, pages 25 to 26, page 649, right column, page 873     Filter ~ 650 page left column     Dye, ultraviolet     Line absorber 6. Binder 26 pages 651 pages left column 873 to 874 pages 7. Plasticizer, page 27, page 650, right column, page 876     lubricant 8. Coating aid, pages 26 to 27, page 650, right column, pages 875 to 876     Surfactant 9. Static 27 pages 650 pages right column 876-877 pages         Preventive agent Ten. Matting agent pp. 878-879.

Although various dye-forming couplers can be used in the light-sensitive material, the following couplers are particularly preferable. Yellow couplers: couplers represented by formulas (I) and (II) of EP 502,424A; couplers represented by formulas (1) and (2) of EP 513,496A (particularly Y-28 on page 18); EP 568,037A Claim 1
A coupler represented by the formula (I) in US Pat. No. 5,066,576, column 1, lines 45 to 55; a coupler represented by the formula (I) in JP-A-4-274425; Couplers; couplers according to claim 1 of EP 498,381A1 on page 40 (especially D-35 on page 18); formulas on page 4 of EP 447,969A1
A coupler represented by (Y) (especially Y-1 (page 17), Y-54 (41
)); US 4,476,219, column 7, lines 36-58, formulas (II)-(I
V) couplers (especially II-17, 19 (column 17), II
-24 (column 19)).

Magenta coupler; JP-A-3-39737
(L-57 (bottom right of page 11), L-68 (bottom right of page 12), L-77 (bottom right of page 13);
EP 456,257, A-4 -63 (page 134), A-4 -73, -75 (page 139);
EP 486,965 M-4, -6 (page 26), M-7 (page 27); EP 571,959A
M-45 (page 19); JP-A-5-204106 (M-1) (page 6); JP-A-4-362631, paragraph 0237, M-22. Cyan coupler: CX-1,3,4,5,1 of JP-A-4-204843
1,12,14,15 (pages 14 to 16); C-7, JP-A-4-43345.
10 (page 35), 34, 35 (37), (I-1), (I-17) (pages 42 to 43); General formula (Ia) of claim 1 of JP-A-6-67385 or (Ib)
A coupler represented by. Polymer coupler: P-1, P-5 (11 in JP-A-2-44345)
page). Examples of couplers in which the coloring dye has an appropriate diffusibility include US 4,366,237, GB 2,125,570, EP 96,873B, DE 3,2
Those described in 34,533 are preferable. The coupler for correcting the unwanted absorption of the color forming dye is a yellow-colored cyan coupler represented by the formulas (CI), (CII), (CIII) and (CIV) described on page 5 of EP 456,257A1 (especially on page 84). YC-86), the yellow colored magenta coupler ExM-7 (page 202) described in the EP,
EX-1 (page 249), EX-7 (page 251), magenta colored cyan coupler CC-9 (column 8), CC described in US 4,833,069
-13 (column 10), US 4,837,136 (2) (column 8), WO92 / 1
The colorless masking couplers of formula (A) of claim 1 of 1575 (in particular the exemplified compounds on pages 36 to 45) are preferred.

Examples of the coupler releasing a photographically useful group include the following. Development inhibitor releasing compound:
Compounds represented by formulas (I), (II), (III) and (IV) described on page 11 of EP 378, 236A1 (particularly T-101 (page 30), T-104 (page 31), T-11
3 (36 pages), T-131 (45 pages), T-144 (51 pages), T-158 (58 pages)), EP 4
Compounds represented by formula (I) on page 7 of 36,938A2 (especially D-49 (page 51)), compounds represented by formula (1) of EP 568,037A (especially (23) (page 11)), Compounds represented by formulas (I), (II) and (III) described on pages 5 to 6 of EP 440,195A2 (especially on page 29)
I- (1)); Bleach accelerator releasing compounds: compounds represented by formulas (I) and (I ') on page 5 of EP 310,125A2 (particularly (60) and (6 on page 61)
1)) and a compound represented by formula (I) in claim 1 of JP-A-6-59411 (particularly (7) (page 7); Ligand releasing compound: LIG-X described in claim 1 of US 4,555,478 Compounds represented (especially compounds on lines 21 to 41 of column 12); Leuco dye releasing compounds: compounds 1 to 6 of columns 3 to 8 of US 4,749,641; fluorescent dye releasing compounds: COUP-DYE of claim 1 of US 4,774,181 Compounds represented (especially columns 7-10)
Compounds 1 to 11); development accelerator or fogging agent releasing compounds: compounds represented by formulas (1), (2) and (3) of column 3, US Pat. No. 4,656,123 (particularly (I-22) of column 25) and EP 450,6
ExZK-2 on page 75, lines 36-38 of 37A2; Compounds that release a dye group only upon leaving: a compound of formula (I) of claim 1 of US 4,857,447 (especially Y- of columns 25-36). 1 ~
Y-19).

As the additives other than the coupler, the following are preferable. Dispersion medium of oil-soluble organic compound: JP-A-62-215272
P-3,5,16,19,25,30,42,49,54,55,66,81,85,86,93 (140〜
(P. 144); Latex for impregnation of oil-soluble organic compounds: US
Latex as described in 4,199,363; Oxidized developer scavenger: Formula (I) in columns 2, lines 54-62 of US 4,978,606.
A compound represented by the formula (especially I-, (1), (2), (6), (12) (columns 4 to 5), a formula of column 5 to line 10 of US Pat. No. 4,923,787 (particularly compound 1 (column 3) ); Antistain agent: EP 298
321A, page 4, lines 30-33, formulas (I)-(III), especially I-47,72, III-
1,27 (pages 24-48); Anti-fading agents: EP 298321A, A-6,7,2
0,21,23,24,25,26,30,37,40,42,48,63,90,92,94,164 (69
~ 118), US 5,122,444 columns 25-38 II-1 ~ III-2
3, especially III-10, EP 471347A, pages 8-12, I-1 to III-4,
II-2, US 5,139,931 columns 32-40, A-1 to 48, especially A-39,42; to reduce the use of color enhancers or color-mixing inhibitors Materials: EP 411324A, pages 5-24 I -1 ~ II-15, especially I-46; Formalin Scavenger: EP 477932A 24 ~
SCV-1 to 28 on page 29, especially SCV-8; Hardener: JP-A 1-21484
Column 1 of H-1,4,6,8,14, US 4,618,573 on page 17 of the publication No. 5
Compounds (H-1 to 5) represented by formulas (VII) to (XII) of 3 to 23
4), Compounds (H-1 to 76) represented by the formula (6) at the lower right of page 8 of JP-A-2-214852, particularly compounds described in claim 1 of H-14, US 3,325,287; Development inhibitor Precursor: JP Sho
62-168139, P-24,37,39 (pages 6-7); US 5,019,49
2 a compound as claimed in claim 1, especially column 7, 28,29;
Preservatives, fungicides: US 4,923,790 columns 3 to 15 I-1
~ III-43, especially II-1,9,10,18, III-25; Stabilizers, antifoggants: US 4,923,793, columns 6 to 16 I-1 to (14), especially I-1,60, (2), (13), US 4,952,483, columns 25-32, compounds 1-65, especially 36: chemical sensitizer: triphenylphosphine selenide, compound 50 of JP-A-5-40324; dye: JP-A-3 -156450, pages 15-18, a-1 to b-20, especially a-1,12,18,27,35,36, b-5,27-29, V-1 to 23, especially
V-1, EP 445627A, FI-1 to F-II-43, especially F- on pages 33 to 55
I-11, F-II-8, EP 457153A, pages 17 to 28, III-1 to 36, particularly III-1,3, WO 88/04794, 8 to 26, Dye-1 to 124, microcrystalline dispersion Compounds 1 to 22 on pages 6 to 11 of EP 319999A, especially compound 1, compounds D-1 to 87 (pages 3 to 28) represented by formulas (1) to (3) of EP 519306A, formula (US Pat. No. 4,268,622) Compounds 1 to 22 represented by I) (columns 3 to 10), compounds represented by formula (I) of US 4,923,788 (1) to (31) (columns 2 to 9);
UV absorber: Compounds (18b) to (18r), 101 to 427 (pages 6 to 9) represented by formula (1) of JP-A-46-3335, EP 520938A
Compounds (3) to (66) (pages 10 to 44) represented by Formula (I) and compounds HBT-1 to 10 (page 14), represented by Formula (III), EP
Compounds (1) to (31) represented by the formula (1) of 521823A (columns 2 to 9).

It can be applied to various color light-sensitive materials such as color negative films for general use or movies, color reversal films for slides or televisions, color papers, color positive films and color reversal papers. In addition, Japanese Patent Publication No.
It is suitable for the film unit with a lens described in Japanese Patent No. 39784.

[0024]

EXAMPLES The present invention will be described below with reference to examples, but the present invention is not limited thereto. [Embodiment] The apparatus shown in FIG. 1 is a method for dissolving the gel-like material for a photographic light-sensitive material of the present invention and an example of the construction of the apparatus. FIG. 1 shows a dissolution apparatus, which is a dissolution tank 2 for dissolving a gel substance. The melting tank 2 has a stirring device 8 for assisting the melting, and by stirring, the heat transfer efficiency of the wall surface of the tank can be improved. Further, the melting tank 2 has a jacket structure, and the heat exchange medium is supplied to the melting tank 2 from a constant temperature bath 3 for conducting heat transfer for melting. The gel substance dissolved in this tank is kept at a predetermined temperature by a temperature sensor 4 provided in the middle of the pipe to be sent to the next step and a heat insulation jacket pipe having a built-in static mixer to measure the dissolution rate. Dissolution rate measuring device 6 for
To measure the dissolution rate. In this device, the dissolution rate and the temperature of the liquid flowing out of the tank are measured in order to bring the dissolution rate to a predetermined rate, and the temperature of the constant temperature bath and / or the rotation speed of the stirrer are controlled according to these signals to determine the dissolution flow rate. Is a device for controlling the. Using the above-mentioned device, dissolution was carried out by controlling the tank temperature keeping conditions and stirring conditions so that the dissolution rate was 2 liters / min. The lower limit of the melting temperature of the thermostatic bath was 26 ° C at which the charged gel substance started sol-gel conversion, and the controllable range was 52 ° C at which the physical properties changed. Further, the stirrer was controlled according to a previously assumed arithmetic expression, with the control range being at least 0 rpm to 60 rpm. As a result, a target flow rate of 2.0 ± 0.2 until the completion of melting of all the amount charged in the tank (about 150 minutes)
It was possible to dissolve with an accuracy within l / min.

[Comparative Example] As a conventional method, 300 kg of a gel-like substance was charged into a 300 kg scale dissolution tank,
Lysis was performed. At this time, the melting temperature was set to 45 ° C.
When the dissolution rate at this time was measured, it was found to be 3 liters / minute at the start of dissolution, but the remaining amount in the tank was reduced to 1.2 liters / minute at 150 kg and to 0.5 liters / minute at 50 kg. I got it.

[0026]

As described above, the method and apparatus for dissolving a gel-like material for a photographic light-sensitive material of the present invention dissolves a gel-like material to be used as a photographic light-sensitive material by using the above-mentioned dissolving device. By controlling the temperature and flow rate to control the melting jacket temperature, it is possible to dissolve at a constant rate, and the changes in photographic performance and physical properties (viscosity, pH, conductivity, etc.) of the dissolved liquid can be made constant. It was possible to obtain a very effective merit in practical use, such as the fact that it became possible to dissolve at a constant rate even if the amount of the gel-like material in the dissolution tank became small.

[Brief description of drawings]

FIG. 1 is a schematic diagram of an apparatus showing one embodiment of the method of the present invention.

[Explanation of symbols]

1 Dissolution device 2 Melting tank 3 heat transfer system 4 temperature sensor 5 heat exchanger 6 Dissolution rate measuring device 7 Thermal insulation jacket 8 stirrer 9 Transfer pipe

Claims (5)

[Claims] 1. A dissolution method in which a gel material used as a photographic light-sensitive material is heated by a jacket in a dissolution tank, or heated by a jacket in a dissolution tank and accelerated by heat transfer by a stirring means. Disposing the means for detecting the temperature at the outlet of the dissolution tank or immediately after the dissolution tank, and the step of using the dissolved gel-like material, or the means for measuring the dissolution rate in the middle of the pipe, the melted gel-like material flowing A method for dissolving a gel-like substance for a photographic light-sensitive material, which comprises adjusting and controlling a heat retention temperature of a dissolution tank jacket according to a flow rate signal and / or a temperature signal of the substance. 2. The method for dissolving a gel-like material for a photographic light-sensitive material according to claim 1, wherein the temperature dependence of the photographic performance and physical properties (viscosity, pH, conductivity, etc.) of the gel-like substance is measured and evaluated in advance. The temperature of the heat medium supplied to the jacket of the dissolution tank is adjusted so that the temperature of the eluting gel-like substance becomes the specified temperature, with the upper limit of the temperature that does not cause adverse effects due to the high temperature of the eluting gel-like substance. Then, the method for dissolving a gel-like substance for a photographic light-sensitive material is characterized in that it is dissolved while controlling the heat retention temperature. 3. The method for dissolving a gel-like material for a photographic light-sensitive material according to claim 1, wherein the dissolution temperature is lowered when the dissolution rate measurement result is faster than the dissolution rate required in the next step. The method for dissolving a gel-like substance for a photographic light-sensitive material is characterized by controlling the temperature in a direction and increasing the temperature when the dissolution rate is insufficient. 4. The method for dissolving a gel-like material for a photographic light-sensitive material according to claim 3, wherein the temperature of the heat medium supplied to the jacket of the dissolution tank is controlled when the dissolution rate is insufficient, and / or the temperature. A method for dissolving a gel-like material for a photographic light-sensitive material, characterized in that the heating medium supply rate required for the jacket is controlled independently. 5. A melting device for melting a gel-like material used as a photographic light-sensitive material, comprising a jacket or a dissolution tank equipped with a jacket and a stirring means, and at the outlet of the dissolution tank or immediately after the dissolution tank According to the flow rate signal of the dissolved gel-like material flowing, and / or the temperature signal, the step of using the dissolved gel-like material, or the means for measuring the dissolution rate is arranged in the middle of the piping. A device for dissolving a gel-like material for a photographic light-sensitive material, characterized in that means for adjusting and controlling the heat retention temperature of the tank jacket is arranged.