EP0507795B1 - Method for de-aerating from an aqueous composition and device for implementing the method - Google Patents
Method for de-aerating from an aqueous composition and device for implementing the method Download PDFInfo
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- EP0507795B1 EP0507795B1 EP91900839A EP91900839A EP0507795B1 EP 0507795 B1 EP0507795 B1 EP 0507795B1 EP 91900839 A EP91900839 A EP 91900839A EP 91900839 A EP91900839 A EP 91900839A EP 0507795 B1 EP0507795 B1 EP 0507795B1
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- mixture
- pressure
- composition
- liquid
- photographic
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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
- G03C1/00—Photosensitive materials
- G03C1/74—Applying photosensitive compositions to the base; Drying processes therefor
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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
- G03C1/00—Photosensitive materials
- G03C1/005—Silver halide emulsions; Preparation thereof; Physical treatment thereof; Incorporation of additives therein
- G03C1/025—Physical treatment of emulsions, e.g. by ultrasonics, refrigeration, pressure
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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
- G03C1/00—Photosensitive materials
- G03C1/74—Applying photosensitive compositions to the base; Drying processes therefor
- G03C2001/7437—Degassing means
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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
- G03C1/00—Photosensitive materials
- G03C1/74—Applying photosensitive compositions to the base; Drying processes therefor
- G03C2001/744—Delivering means for slide hopper
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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
- G03C2200/00—Details
- G03C2200/09—Apparatus
Definitions
- the invention relates to an apparatus and a method for degassing substances, in particular emulsions obtained from pieces of frozen photographic emulsion.
- a method and a device are known for subjecting a liquid, with which a gas is simultaneously supplied, to a first degassing under vacuum while, in a second phase, this liquid is degassed further by means of a centrifugal rotor, to then accumulate in the form of an annular layer of liquid in a pumping element and then to be expelled by centrifugal forces against the vacuum prevailing in the system .
- a device for degassing liquids is known, a device in which the liquid is treated under vacuum in a centrifuge, this liquid spreading into a flowing film on the inner wall of the centrifuge rotor, to then be distributed into a fraction low in bubbles and a fraction rich in bubbles. So that the bubble-rich fraction can then be separated from the bubble-poor fraction, at the point where the liquid leaves the rotor while going outwards, a blade-shaped overflow element is provided on a on which side passes the liquid rich in bubbles, which is again introduced into the rotor to be treated there while, on the other side, the liquid is evacuated at a peripheral speed decreasing, this liquid having to be relatively poor in bubbles . In fact, compared to the liquid which is introduced into the rotor before degassing, the liquid discharged there is poorer in bubbles, but a sufficient absence of bubbles is not achieved.
- stage (1) The constituents prepared separately in stage (1) can be kept cold separately, either after stage (1), or after stage (2) in the form of pieces, or at the same time after stage (1 ) and after step (2).
- the average volume of the pieces must not exceed 2 cm3, so as to ensure the homogeneity of the mixture in the subsequent solid state, and it is preferably less than 0.5 cm3.
- the composition is liquefied by means of a device comprising for example an archimedean screw and a pump passing the solid composition in a heat exchanger.
- a deaeration device such as that described in application EP-A-58 353.
- EP-A -58,353 describes a method and an apparatus in which the liquid is spread in a thin film by subjecting it to a sudden depression.
- the pressure in absolute value to which the liquid film is subjected is of the order of 8100 Pa. But under these pressure conditions, even if the formation of bubbles is reduced, the molten emulsion contains a large amount of dissolved air at a rate almost reaching saturation.
- the objects of the present invention are achieved by a deaeration process of a mixture of various constituents of an aqueous composition, in the form of solid pieces, characterized in that one applies to the mixture and before recasting of said mixture a pressure close to the water vapor pressure corresponding to the temperature of said mixture, said solid pieces having a volume less than or equal to 2.0 cm3.
- the invention also relates to a device for supplying a photographic coating station at which a liquid photographic composition is applied to a support, characterized in that it comprises means (4, 9, 10) allowing the setting work of the method according to any one of claims 1 to 5 and arranged just upstream of the remelting device supplying said coating station.
- the device shown in FIG. 1 mainly comprises a feed hopper 1, a deaeration device 4, conveyor devices 2 and 3 for transporting the mixture and a remelting device 5.
- the feed hopper (1) is fed with a mixture of various constituents of an aqueous composition, in the form of solid pieces.
- this mixture consists of a photographic composition with silver halides, capable of being applied on a support to form a layer.
- the process for obtaining these solid pieces consists, as described in patent application FR-A-2 626 088, of separately preparing the various constituents of the layer to be obtained, comprising at least one emulsion with silver halides, and solutions or dispersions containing one or more of the finishing additives and / or gelatin, to cool these constituents, to solidify them each in the solid state, to cut them into pieces, to mix in the cold, solid state, the constituents chosen according to the formulation of the desired layer.
- the feed hopper is provided at its base with a device with rotating blades (8) to prevent the formation of a bridge at the outlet of said hopper.
- the first device (2) transports the mixture from the feed hopper (1) to the deaeration device (4) which will be discussed in more detail later.
- the second ensures the transport of the mixture from the deaeration device (4) to a device for recasting the mixture (5) which will also be discussed in detail later.
- these conveying devices consist of a conventional Archimedes screw. These two Archimedes screws (2), (3) are rotated by the respective motors (6) and (7) and terminate respectively by a sealed device (13) which can be, for example a pump of the MOINEAU type .
- a deaeration device consisting of a vacuum enclosure (4) between the two conveying devices and upstream of the device for recasting (5) of the mixture. Inside this enclosure, a pressure close to the water vapor pressure corresponding to the temperature of the mixture is applied to the mixture, said enclosure comprising an inlet orifice through which the solid mixture coming from the feed hopper and driven by said first conveying device (2) is introduced into said vacuum enclosure (4) and an outlet orifice through which the solid mixture is evacuated from said enclosure and is driven by means of said second device conveying (3) to the mixture redesign device (5).
- the absolute pressure inside the depression chamber is between 1000 and 2000 Pa and preferably is between 1000 and 1500 Pa.
- the depression chamber (4) is, according to one embodiment, put in depression by means of a pump (9) connected to the enclosure by a tube (10).
- the enclosure (4) is provided with a stirring device (11) with rotary blades.
- the conveying device (3) and the stirring device (11) are rotatably mounted by means of bearings (not shown) allowing the enclosure (4) to be placed under vacuum.
- the role of this vacuum enclosure (4) is to minimize the amount of interstitial air (that is to say, between the pieces forming the mixture) and to decrease the amount of air dissolved in the composition it -even.
- the device for recasting the mixture (5) is located downstream of the vacuum enclosure and comprises a heat exchanger supplied, for example, by a circulation (14) of a thermal liquid.
- the emulsion is remelted at around 40 ° C and exits through the pipe (15).
- the heat exchanger is of the multitubular type. Its exchange surface is 3.2 m2.
- the heating fluid is water, the temperature of which is adjusted as a function of the flow rate of composition to be melted, but preferably less than 60 ° C. to ensure more regular reheating.
- the motor driving the conveying device (3) in rotation is controlled by the flow rate of the molten mixture leaving through the pipe (15).
- the motor driving the conveying device (2) in rotation can be controlled by the volume contained in the vacuum enclosure (4) by means of a probe (16). It is also possible to use an alarm device (17) indicating an insufficient filling level of the feed hopper (1).
- a photographic dispersion similar to that used for color paper is used.
- the viscosity of the composition once melted is of the order of 100 cp at 40 ° C.
- the speed of the Archimedes' screws is adjusted so as to obtain a dispersion rate once liquefied of 4 l / min.
- the absolute pressure of enclosure 4 is adjusted to a value of 1500 Pa.
- a gelatin broth containing 15% dry gelatin is used.
- the flow rate is 4 l / min and the pressure is 1500 Pa.
- the viscosity of the composition once melted is of the order of 70 cp at 40 ° C.
- Dissolved oxygen is 1.4 ppm at 40 ° C.
- a gelatin broth containing 7% dry gelatin is used.
- the flow rate is 12 l / min and the pressure between 1200 Pa and 1400 Pa.
- the viscosity of the composition once melted is of the order of 7 cp at 40 ° C.
- the dissolved oxygen is equal to 3.2 ppm at 40 ° C and the entrained air rate at 0.01%.
- Example 3 The same composition is used as that used in Example 3 but this time no vacuum is applied inside the enclosure 4.
- the dissolved oxygen is equal to 6.3 ppm at 40 ° C (saturation) and the entrained air rate is 5%.
Abstract
Description
L'invention concerne un appareil et un procédé de dégazage de substances, en particulier d'émulsions obtenues à partir de morceaux d'émulsion photographique figée.The invention relates to an apparatus and a method for degassing substances, in particular emulsions obtained from pieces of frozen photographic emulsion.
Bon nombre de produits de l'industrie chimique, de l'industrie pharmaceutique, de l'industrie des produits alimentaires et des industries connexes, en particulier, des émulsions, des suspensions, des pâtes et des liquides de haute viscosité ou analogues contiennent de l'air ou des gaz dissous ou sous forme de petites bulles qui, lors de la fabrication, viennent inévitablement s'incorporer dans le liquide, mais qui ne doivent se trouver dans le produit final. C'est ainsi que, par exemple, dans le cas des émulsions photographiques, les bulles de gaz altèrent dans une importante mesure la qualité des pellicules ou des papiers photographiques réalisés avec ces émulsions du fait que les bulles ou les petites bulles de gaz perturbent le courant volumique dans les dispositifs d'enduction, donnant ainsi lieu à la formation de rayures qui rendent les matériaux photographiques inutilisables.Many products of the chemical, pharmaceutical, food and related industries, in particular, emulsions, suspensions, pastes and high viscosity liquids or the like contain l air or gases dissolved or in the form of small bubbles which, during manufacture, inevitably become incorporated into the liquid, but which must not be present in the final product. Thus, for example, in the case of photographic emulsions, the gas bubbles significantly affect the quality of the films or photographic paper produced with these emulsions because the bubbles or small gas bubbles disturb the volume current in coating devices, thus giving rise to the formation of scratches which render photographic materials unusable.
D'après le brevet GB-A-2 008 971, on connaît un procédé et un dispositif permettant de soumettre un liquide, avec lequel est simultanément acheminé un gaz, à un premier dégazage sous dépression tandis que, dans une deuxième phase, ce liquide est dégazé davantage au moyen d'un rotor centrifuge, pour s'accumuler ensuite sous forme d'une couche annulaire de liquide dans un élément de pompage et pour être ensuite expulsé par des forces centrifuges à l'encontre de la dépression régnant dans le système.According to patent GB-A-2 008 971, a method and a device are known for subjecting a liquid, with which a gas is simultaneously supplied, to a first degassing under vacuum while, in a second phase, this liquid is degassed further by means of a centrifugal rotor, to then accumulate in the form of an annular layer of liquid in a pumping element and then to be expelled by centrifugal forces against the vacuum prevailing in the system .
Ce dispositif et ce procédé présentent des inconvénients importants, car le liquide s'accumule et s'écoule entre le rotor centrifuge et les parois du logement, ainsi qu'entre les rotors des pompes et les parois, ce liquide étant ainsi exposé à d'importantes forces de cisaillement. De la sorte, la friction provoque un dégagement de chaleur qui n'est pas contrôlable. La chaleur dégagée conduit à la formation d'agrégats incrustés et, lorsque ces derniers se détachent, ils forment de petits grumeaux qui, dans le cas d'émulsions photographiques, présentent des inconvénients plus importants encore que de petites bulles. Dans le cas d'un échauffement trop important, la qualité de l'émulsion photographique en souffre dans une importante mesure. Par suite de la sortie du liquide à la périphérie de la pompe, il se produit, dans l'écoulement, d'importantes perturbations qui peuvent à nouveau conduire à la formation de petites bulles.This device and this method have significant drawbacks, since the liquid collects and flows between the centrifugal rotor and the walls of the housing, as well as between the pump rotors and the walls, this liquid being thus exposed to significant shear forces. In this way, friction causes the generation of heat which is not controllable. The heat released leads to the formation of encrusted aggregates and, when the latter are detached, they form small lumps which, in the case of photographic emulsions, have even greater disadvantages than small bubbles. In the event of excessive heating, the quality of the photographic emulsion suffers to a great extent. As a result of the liquid leaving the periphery of the pump, significant disturbances occur in the flow which can again lead to the formation of small bubbles.
De même, d'après le brevet DE-C-2 147 124, on connaît un dispositif de dégazage de liquides, dispositif dans lequel le liquide est traité sous vide dans une centrifugeuse, ce liquide s'étalant en une pellicule qui s'écoule sur la paroi intérieure du rotor de la centrifugeuse, pour être ensuite réparti en une fraction pauvre en bulles et une fraction riche en bulles. Afin que la fraction riche en bulles puisse alors être séparée de la fraction pauvre en bulles, à l'endroit où le liquide quitte le rotor en se dirigeant vers l'extérieur, on prévoit un élément de trop-plein en forme de lame sur un côté duquel passe le liquide riche en bulles, qui est à nouveau introduit dans le rotor pour y être traité tandis que, de l'autre côté, le liquide est évacué à une vitesse périphérique allant en diminuant, ce liquide devant être relativement pauvre en bulles. En fait, comparativement au liquide qui est introduit dans le rotor avant le dégazage, le liquide évacué à cet endroit est plus pauvre en bulles, mais on n'atteint pas une absence de bulles suffisante.Likewise, according to patent DE-C-2 147 124, a device for degassing liquids is known, a device in which the liquid is treated under vacuum in a centrifuge, this liquid spreading into a flowing film on the inner wall of the centrifuge rotor, to then be distributed into a fraction low in bubbles and a fraction rich in bubbles. So that the bubble-rich fraction can then be separated from the bubble-poor fraction, at the point where the liquid leaves the rotor while going outwards, a blade-shaped overflow element is provided on a on which side passes the liquid rich in bubbles, which is again introduced into the rotor to be treated there while, on the other side, the liquid is evacuated at a peripheral speed decreasing, this liquid having to be relatively poor in bubbles . In fact, compared to the liquid which is introduced into the rotor before degassing, the liquid discharged there is poorer in bubbles, but a sufficient absence of bubbles is not achieved.
Toutes ces techniques concernent en réalité le dégazage de substances à l'état liquide. Or depuis quelques temps, en particulier dans le domaine des produits photographiques, les techniques de fabrication de l'émulsion utilisent des mélanges au froid et à l'état figé solide des divers constituants d'une composition aqueuse de couchage.All these techniques actually relate to the degassing of substances in the liquid state. Gold for some time, especially in the area of products Photographic, emulsion manufacturing techniques use mixtures of cold and solid frozen state of the various constituents of an aqueous coating composition.
Ainsi, la demande de brevet FR-A-2 626 088 décrit un procédé d'obtention d'une composition photographique apte à former une couche sur un support, ladite composition contenant au moins une émulsion aux halogénures d'argent, ainsi que les additifs chimiques de finition nécessaires. Le procédé suivant cette demande consiste à :
- 1) préparer séparément, ou par groupe de composés compatibles, divers constituants de la couche souhaitée, comprenant au moins une émulsion aux halogénures d'argent et des solutions ou des dispersions contenant un ou plusieurs des additifs de finition et/ou de la gélatine, et refroidir ces constituants, pour les figer chacun à l'état solide,
- 2) les couper en morceaux,
- 3) mélanger au froid, à l'état solide, les constituants choisis en fonction de la formulation de la couche souhaitée, ou d'une partie de cette couche,
- 4) liquéfier la composition solide obtenue en vue de son introduction dans le poste d'enduction.
- 1) preparing separately, or by group of compatible compounds, various constituents of the desired layer, comprising at least one silver halide emulsion and solutions or dispersions containing one or more of the finishing additives and / or gelatin, and cool these constituents, to freeze them each in the solid state,
- 2) cut them into pieces,
- 3) mix in the cold, in the solid state, the constituents chosen according to the formulation of the desired layer, or of a part of this layer,
- 4) liquefying the solid composition obtained with a view to its introduction into the coating station.
Les constituants préparés séparément à l'étape (1) peuvent être conservés au froid séparément, soit après l'étape (1), soit après l'étape (2) sous forme de morceaux, soit à la fois après l'étape (1) et après l'étape (2).The constituents prepared separately in stage (1) can be kept cold separately, either after stage (1), or after stage (2) in the form of pieces, or at the same time after stage (1 ) and after step (2).
Le volume moyen des morceaux ne doit pas dépasser 2 cm³, de façon à assurer l'homogénéité du mélange à l'état solide subséquent, et il est de préférence inférieur à 0,5 cm³.The average volume of the pieces must not exceed 2 cm³, so as to ensure the homogeneity of the mixture in the subsequent solid state, and it is preferably less than 0.5 cm³.
Dans cette demande de brevet, la composition est liquéfiée au moyen d'un dispositif comportant par exemple une vis d'archimède et une pompe faisant passer la composition solide dans un échangeur de chaleur. Cependant avec un tel procédé, afin d'éviter les bulles à la sortie de l'émulsion fondue, il faut mettre en oeuvre un dispositif de désaération, tel que celui décrit dans la demande EP-A-58 353. Cette demande EP-A-58 353 décrit un procédé et un appareil dans lequel on étale le liquide en une mince pellicule en lui faisant subir une brusque dépression. La pression en valeur absolue à laquelle on soumet la pellicule de liquide est de l'ordre de 8100 Pa. Mais dans ces conditions de pression, même si on réduit la formation de bulles, l'émulsion fondue comporte une grande quantité d'air dissous selon un taux atteignant pratiquement la saturation.In this patent application, the composition is liquefied by means of a device comprising for example an archimedean screw and a pump passing the solid composition in a heat exchanger. However, with such a method, in order to avoid bubbles at the outlet of the molten emulsion, it is necessary to use a deaeration device, such as that described in application EP-A-58 353. This application EP-A -58,353 describes a method and an apparatus in which the liquid is spread in a thin film by subjecting it to a sudden depression. The pressure in absolute value to which the liquid film is subjected is of the order of 8100 Pa. But under these pressure conditions, even if the formation of bubbles is reduced, the molten emulsion contains a large amount of dissolved air at a rate almost reaching saturation.
Les brevets US-A-3 797 551 et CH-B-500 507 décrivent un procédé de solidification d'émulsions de gélatine dans lequel on applique aux émulsions liquides une dépression comprise entre 933 et 1560 Pa à environ 11°C. Un tel procédé pose des problèmes relatifs à la variation de la concentration des émulsions due à la quantité relativement importante d'eau qui est enlevée du produit par évaporation sous vide.The patents US-A-3 797 551 and CH-B-500 507 describe a process for solidifying gelatin emulsions in which a vacuum of between 933 and 1560 Pa is applied to liquid emulsions at about 11 ° C. Such a method poses problems relating to the variation in the concentration of the emulsions due to the relatively large amount of water which is removed from the product by evaporation under vacuum.
Aussi est-ce un des objets de la présente invention que d'améliorer la désaération d'une composition avant de l'envoyer au poste d'enduction.It is therefore one of the objects of the present invention to improve the deaeration of a composition before sending it to the coating station.
C'est encore un autre objet de la présente invention que de réaliser un dispositif de désaération plus simple et plus fiable que ceux utilisés jusqu'a présent dans la technique.It is yet another object of the present invention to provide a simpler and more reliable deaeration device than those used hitherto in the art.
C'est encore un autre objet de la présente invention, que de réduire au minimum la quantité d'air intersticiel c'est-à-dire entre les morceaux solides) et de diminuer également la quantité d'air dissous dans la composition elle même.It is yet another object of the present invention, to minimize the amount of interstitial air (i.e. between the solid pieces) and also to decrease the amount of air dissolved in the composition itself .
D'autres objets apparaitront au cours de la description plus détaillée qui suit.Other objects will appear during the more detailed description which follows.
Les objets de la présente invention sont réalisés par un procédé de désaération d'un mélange de divers constituants d'une composition aqueuse, sous forme de morceaux solides, caractérisé en ce que l'on applique au mélange et avant refonte dudit mélange une pression voisine de la tension de vapeur d'eau correspondant à la température dudit mélange, lesdits morceaux solides ayant un volume inférieur ou égal à 2.0 cm³.The objects of the present invention are achieved by a deaeration process of a mixture of various constituents of an aqueous composition, in the form of solid pieces, characterized in that one applies to the mixture and before recasting of said mixture a pressure close to the water vapor pressure corresponding to the temperature of said mixture, said solid pieces having a volume less than or equal to 2.0 cm³.
L'invention concerne également un dispositif d'alimentation d'un poste d'enduction photographique au niveau duquel une composition photographique liquide est appliquée sur un support caractérisé en ce qu'il comprend des moyens (4, 9, 10) permettant la mise en oeuvre du procédé selon l'une quelconque des revendications 1 à 5 et disposés juste en amont du dispositif de refonte alimentant ledit poste d'enduction.The invention also relates to a device for supplying a photographic coating station at which a liquid photographic composition is applied to a support, characterized in that it comprises means (4, 9, 10) allowing the setting work of the method according to any one of claims 1 to 5 and arranged just upstream of the remelting device supplying said coating station.
La description plus détaillée qui suit sera illustrée en faisant référence à une unique figure représentant un dispositif de liquéfaction comprenant un dispositif de désaération selon la présente invention.The more detailed description which follows will be illustrated with reference to a single figure representing a liquefaction device comprising a deaeration device according to the present invention.
Le dispositif représenté en Fig. 1 comprend principalement une trémie d'alimentation 1, un dispositif de désaération 4, des dispositifs de convoyage 2 et 3 pour transporter le mélange et un dispositif de refonte 5.The device shown in FIG. 1 mainly comprises a feed hopper 1, a deaeration device 4,
On alimente la trémie d'alimentation (1) avec un mélange de divers constituants d'une composition aqueuse, sous forme de morceaux solides. Dans un mode de réalisation particulier, ce mélange consiste en une composition photographique aux halogénures d'argent, apte à être appliquée sur un support pour former une couche. Le procédé d'obtention de ces morceaux solides consiste, ainsi que décrit dans la demande de brevet FR-A-2 626 088, à préparer séparément les divers constituants de la couche à obtenir, comprenant au moins une émulsion aux halogénures d'argent, et des solutions ou des dispersions contenant un ou plusieurs des additifs de finition et/ou de la gélatine, à refroidir ces constituants, pour les figer chacun à l'état solide, à les couper en morceaux, à mélanger au froid, à l'état solide, les constituants choisis en fonction de la formulation de la couche désirée. La trémie d'alimentation est munie à sa base d'un dispositif à pales rotatives (8) pour éviter la formation d'un pont à la sortie de ladite trémie.The feed hopper (1) is fed with a mixture of various constituents of an aqueous composition, in the form of solid pieces. In a particular embodiment, this mixture consists of a photographic composition with silver halides, capable of being applied on a support to form a layer. The process for obtaining these solid pieces consists, as described in patent application FR-A-2 626 088, of separately preparing the various constituents of the layer to be obtained, comprising at least one emulsion with silver halides, and solutions or dispersions containing one or more of the finishing additives and / or gelatin, to cool these constituents, to solidify them each in the solid state, to cut them into pieces, to mix in the cold, solid state, the constituents chosen according to the formulation of the desired layer. The feed hopper is provided at its base with a device with rotating blades (8) to prevent the formation of a bridge at the outlet of said hopper.
Le premier dispositif (2) assure le transport du mélange de la trémie d'alimentation (1) vers le dispositif de désaération (4) dont on reparlera plus en détail par la suite. Le second assure le transport du mélange du dispositif de désaération (4) vers un dispositif de refonte du mélange (5) dont on reparlera également en détail par la suite. Selon un mode de réalisation ces dispositifs de convoyage sont constitués d'une vis d'Archimède conventionnelle. Ces deux vis d'Archimède (2), (3) sont entraînées en rotation par les moteurs respectifs (6) et (7) et se terminent respectivement par un dispositif étanche (13) qui peut être, par exemple une pompe du type MOINEAU.The first device (2) transports the mixture from the feed hopper (1) to the deaeration device (4) which will be discussed in more detail later. The second ensures the transport of the mixture from the deaeration device (4) to a device for recasting the mixture (5) which will also be discussed in detail later. According to one embodiment, these conveying devices consist of a conventional Archimedes screw. These two Archimedes screws (2), (3) are rotated by the respective motors (6) and (7) and terminate respectively by a sealed device (13) which can be, for example a pump of the MOINEAU type .
Suivant l'invention on dispose un dispositif de désaération constitué d'une enceinte de dépression (4) entre les deux dispositifs de convoyage et en amont du dispositif de refonte (5) du mélange. A l'intérieur de cette enceinte on applique au mélange une pression voisine de la tension de vapeur d'eau correspondant à la température du mélange, ladite enceinte comprenant un orifice d'entrée par lequel le mélange solide provenant de la trémie d'alimentation et entraîné par ledit premier dispositif de convoyage (2) est introduit dans ladite enceinte de dépression (4) et un orifice de sortie par lequel le mélange solide est évacué de ladite enceinte et est entraîné au moyen dudit second dispositif de convoyage (3) vers le dispositif de refonte du mélange (5). La pression absolue à l'intérieur de l'enceinte de dépresssion est comprise entre 1000 et 2000 Pa et de préférence est comprise entre 1000 et 1500 Pa. L'enceinte de dépression (4) est, selon un mode de réalisation, mise en dépression par l'intermédiaire d'une pompe (9) reliée à l'enceinte par un tube (10). L'enceinte (4) est munie d'un dispositif de brassage (11) à pales rotatives. Le dispositif de convoyage (3) ainsi que le dispositif de brassage (11) sont montés à rotation par l'intermédiaire de paliers (non représentés) permettant la mise en dépression de l'enceinte (4). Le rôle de cette enceinte de dépression (4) est de réduire au minimum la quantité d'air intersticiel (c'est-à-dire, entre les morceaux formant le mélange) et de diminuer la quantité d'air dissous dans la composition elle-même.According to the invention there is a deaeration device consisting of a vacuum enclosure (4) between the two conveying devices and upstream of the device for recasting (5) of the mixture. Inside this enclosure, a pressure close to the water vapor pressure corresponding to the temperature of the mixture is applied to the mixture, said enclosure comprising an inlet orifice through which the solid mixture coming from the feed hopper and driven by said first conveying device (2) is introduced into said vacuum enclosure (4) and an outlet orifice through which the solid mixture is evacuated from said enclosure and is driven by means of said second device conveying (3) to the mixture redesign device (5). The absolute pressure inside the depression chamber is between 1000 and 2000 Pa and preferably is between 1000 and 1500 Pa. The depression chamber (4) is, according to one embodiment, put in depression by means of a pump (9) connected to the enclosure by a tube (10). The enclosure (4) is provided with a stirring device (11) with rotary blades. The conveying device (3) and the stirring device (11) are rotatably mounted by means of bearings (not shown) allowing the enclosure (4) to be placed under vacuum. The role of this vacuum enclosure (4) is to minimize the amount of interstitial air (that is to say, between the pieces forming the mixture) and to decrease the amount of air dissolved in the composition it -even.
Le dispositif de refonte du mélange (5) est situé en aval de l'enceinte de dépression et comprend un échangeur de chaleur alimenté, par exemple, par une circulation (14) d'un liquide thermique. L'émulsion est refondue à environ 40°C et sort par le tuyau (15). Selon un mode de réalisation particulier l'échangeur de chaleur est du type multitubulaire. Sa surface d'échange est de 3,2 m². Le fluide chauffant est de l'eau dont on ajuste la température en fonction du débit de composition à refondre, mais de préférence inférieure à 60°C pour assurer un réchauffage plus régulier.The device for recasting the mixture (5) is located downstream of the vacuum enclosure and comprises a heat exchanger supplied, for example, by a circulation (14) of a thermal liquid. The emulsion is remelted at around 40 ° C and exits through the pipe (15). According to a particular embodiment, the heat exchanger is of the multitubular type. Its exchange surface is 3.2 m². The heating fluid is water, the temperature of which is adjusted as a function of the flow rate of composition to be melted, but preferably less than 60 ° C. to ensure more regular reheating.
Dans un mode de réalisation préférentiel, le moteur entraînant en rotation le dispositif de convoyage (3) est asservi au débit du mélange fondu sortant par le tuyau (15). De même, le moteur entraînant en rotation le dispositif de convoyage (2) peut être asservi au volume contenu dans l'enceinte de dépression (4) au moyen d'une sonde (16). On peut également utiliser un dispositif d'alarme (17) indiquant un niveau de remplissage insuffisant de la trémie d'alimentation (1).In a preferred embodiment, the motor driving the conveying device (3) in rotation is controlled by the flow rate of the molten mixture leaving through the pipe (15). Similarly, the motor driving the conveying device (2) in rotation can be controlled by the volume contained in the vacuum enclosure (4) by means of a probe (16). It is also possible to use an alarm device (17) indicating an insufficient filling level of the feed hopper (1).
Les essais ont montré que de tels dispositifs étaient susceptibles de fonctionner à des débits pouvant aller de un litre à vingt litres de mélange par minute. Il est possible avec de tels dispositifs de diminuer le taux d'air dissous dans le mélange à moins de 50 % du taux de saturation à la pression atmosphérique. Les essais ont également montré que les meilleurs résultats étaient obtenus pour un temps de passage, du mélange solide dans l'enceinte de dépression, compris entre 5 et 10 mn.Tests have shown that such devices are capable of operating at flow rates ranging from one liter to twenty liters of mixture per minute. It is possible with such devices to reduce the rate of air dissolved in the mixture to less than 50% of the saturation rate at atmospheric pressure. The tests also showed that the best results were obtained for a passage time of the solid mixture in the depression enclosure, between 5 and 10 min.
On utilise un dispersion photographique analogue à celle utilisée pour le papier couleur.A photographic dispersion similar to that used for color paper is used.
La viscosité de la composition une fois fondue est de l'ordre de 100 cp à 40°C.The viscosity of the composition once melted is of the order of 100 cp at 40 ° C.
On règle la vitesse des vis d'Archimède de manière à obtenir un débit de dispersion une fois liquéfiée de 4 l/mn. On règle la pression absolue de l'enceinte 4 à une valeur de 1500 Pa.The speed of the Archimedes' screws is adjusted so as to obtain a dispersion rate once liquefied of 4 l / min. The absolute pressure of enclosure 4 is adjusted to a value of 1500 Pa.
Lorsqu'on a appliqué cette pression à l'enceinte 4, on mesure après refonte à 40°C, le taux d'air entrainé et le taux d'oxygène dissous qui sont respectivement égaux à 0,04 % et 1,6 ppm.When this pressure has been applied to the enclosure 4, the rate of entrained air and the rate of dissolved oxygen, which are equal to 0.04% and 1.6 ppm respectively, are measured after recasting at 40 ° C.
On utilise un bouillon de gélatine à 15 % de gélatine sèche. Le débit est de 4 l/mn et la pression de 1500 Pa. La viscosité de la composition une fois fondue est de l'ordre de 70 cp à 40°C. L'oxygène dissous est égal à 1,4 ppm à 40°C.A gelatin broth containing 15% dry gelatin is used. The flow rate is 4 l / min and the pressure is 1500 Pa. The viscosity of the composition once melted is of the order of 70 cp at 40 ° C. Dissolved oxygen is 1.4 ppm at 40 ° C.
On utilise un bouillon de gélatine à 7 % de gélatine sèche. Le débit est de 12 l/mn et la pression comprise entre 1200 Pa et 1400 Pa. La viscosité de la composition une fois fondue est de l'ordre de 7 cp à 40°C. L'oxygène dissous est égal à 3,2 ppm à 40°C et le taux d'air entraîné à 0,01 %.A gelatin broth containing 7% dry gelatin is used. The flow rate is 12 l / min and the pressure between 1200 Pa and 1400 Pa. The viscosity of the composition once melted is of the order of 7 cp at 40 ° C. The dissolved oxygen is equal to 3.2 ppm at 40 ° C and the entrained air rate at 0.01%.
On utilise la même composition que celle utilisée dans l'exemple 3 mais cette fois on applique aucune dépression à l'intérieur de l'enceinte 4. L'oxygène dissous est égal à 6,3 ppm à 40°C (saturation) et le taux d'air entraîné est de 5 %.The same composition is used as that used in Example 3 but this time no vacuum is applied inside the enclosure 4. The dissolved oxygen is equal to 6.3 ppm at 40 ° C (saturation) and the entrained air rate is 5%.
Claims (6)
- Degassing method for a mixture of various components in an aqueous composition, in the form of solid chunks, characterized in that a pressure near the steam pressure corresponding to the temperature of the mixture is applied, before melting, to said mixture, said solids chunks exhibiting a volume equal to or lower than 2.0 cm3.
- Method according to claim 1, wherein said solids chunks exhibit a volume lower than.5 cm3.
- Method according to claim 1 characterized in that the absolute pressure applied to the mixture ranges from 1000 to 2000 Pa.
- Method according to claim 3 characterized in that the absolute pressure applied to the mixture ranges from 1000 to 1500 Pa.
- Method according to any of the claims 1 to 4, characterized in that the pressure is applied to the mixture before melting for a period of time ranging from 5 to 10 mn.
- Feeding device for a photographic coating machine wherein a liquid photographic composition is deposited on a support, characterized in that it comprises a vacuum chamber (4), a pump (9) connected to said chamber via a pipe (10) as means for operating the process of any of the claims 1 to 5, said feeding device being located just upstream a melting device (5) feeding said coating machine.
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
FR8917515 | 1989-12-26 | ||
FR8917515A FR2656293B1 (en) | 1989-12-26 | 1989-12-26 | PROCESS FOR DEAERATING AN AQUEOUS COMPOSITION AND DEVICE FOR CARRYING OUT THIS PROCESS. |
Publications (2)
Publication Number | Publication Date |
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EP0507795A1 EP0507795A1 (en) | 1992-10-14 |
EP0507795B1 true EP0507795B1 (en) | 1994-02-23 |
Family
ID=9389194
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP91900839A Expired - Lifetime EP0507795B1 (en) | 1989-12-26 | 1991-07-25 | Method for de-aerating from an aqueous composition and device for implementing the method |
Country Status (6)
Country | Link |
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US (1) | US5264024A (en) |
EP (1) | EP0507795B1 (en) |
JP (1) | JPH05503031A (en) |
DE (1) | DE69006858T2 (en) |
FR (1) | FR2656293B1 (en) |
WO (1) | WO1991010164A1 (en) |
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US5275793A (en) * | 1992-08-28 | 1994-01-04 | Eastman Kodak Company | Direct coupled degasser and liquefier |
US6730469B2 (en) * | 2001-07-05 | 2004-05-04 | Fuji Photo Film Co., Ltd. | Method and apparatus for liquid preparation of photographic reagent |
US20070281003A1 (en) | 2001-10-12 | 2007-12-06 | Fuisz Richard C | Polymer-Based Films and Drug Delivery Systems Made Therefrom |
US20110033542A1 (en) | 2009-08-07 | 2011-02-10 | Monosol Rx, Llc | Sublingual and buccal film compositions |
US8603514B2 (en) | 2002-04-11 | 2013-12-10 | Monosol Rx, Llc | Uniform films for rapid dissolve dosage form incorporating taste-masking compositions |
US11207805B2 (en) | 2001-10-12 | 2021-12-28 | Aquestive Therapeutics, Inc. | Process for manufacturing a resulting pharmaceutical film |
US10285910B2 (en) | 2001-10-12 | 2019-05-14 | Aquestive Therapeutics, Inc. | Sublingual and buccal film compositions |
US8765167B2 (en) | 2001-10-12 | 2014-07-01 | Monosol Rx, Llc | Uniform films for rapid-dissolve dosage form incorporating anti-tacking compositions |
US7425292B2 (en) | 2001-10-12 | 2008-09-16 | Monosol Rx, Llc | Thin film with non-self-aggregating uniform heterogeneity and drug delivery systems made therefrom |
US7357891B2 (en) | 2001-10-12 | 2008-04-15 | Monosol Rx, Llc | Process for making an ingestible film |
US8900498B2 (en) | 2001-10-12 | 2014-12-02 | Monosol Rx, Llc | Process for manufacturing a resulting multi-layer pharmaceutical film |
US8900497B2 (en) | 2001-10-12 | 2014-12-02 | Monosol Rx, Llc | Process for making a film having a substantially uniform distribution of components |
US20190328679A1 (en) | 2001-10-12 | 2019-10-31 | Aquestive Therapeutics, Inc. | Uniform films for rapid-dissolve dosage form incorporating anti-tacking compositions |
US9149959B2 (en) | 2010-10-22 | 2015-10-06 | Monosol Rx, Llc | Manufacturing of small film strips |
US11273131B2 (en) | 2016-05-05 | 2022-03-15 | Aquestive Therapeutics, Inc. | Pharmaceutical compositions with enhanced permeation |
BR112018072539A2 (en) | 2016-05-05 | 2019-03-26 | Aquestive Therapeutics, Inc. | increased administration epinephrine compositions |
Family Cites Families (13)
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US2704658A (en) * | 1955-03-22 | Mud agitator | ||
CH500507A (en) * | 1968-12-19 | 1970-12-15 | Agfa Gevaert Ag | Process for the production of bubble-free solidified photoemulsions |
CH564793A5 (en) * | 1970-10-10 | 1975-07-31 | Agfa Gevaert Ag | |
US3797551A (en) * | 1971-07-21 | 1974-03-19 | Agfa Gevaert Ag | Solidification of gelatin emulsions |
DE2147124C3 (en) * | 1971-09-21 | 1974-08-22 | Rumpf, Hans, Prof. Dr.-Ing., 7500 Karlsruhe | Method and device for degassing liquids |
US3793805A (en) * | 1971-12-13 | 1974-02-26 | Eastman Kodak Co | Method and apparatus for removing air from a liquid |
DE2543328B2 (en) * | 1975-09-29 | 1978-01-12 | Paul Troester Maschinenfabrik, 3000 Hannover | DEVICE FOR EXTRUDING THERMOPLASTIC PLASTICS AND ELASTOMERS |
JPS54121728A (en) * | 1978-03-14 | 1979-09-21 | Konishiroku Photo Ind Co Ltd | Sensitization method for silver halide photographic material |
US4318839A (en) * | 1981-01-23 | 1982-03-09 | General Motors Corporation | Polyamide based thermoplastic body solder |
DE3105914A1 (en) * | 1981-02-18 | 1982-09-09 | Agfa-Gevaert Ag, 5090 Leverkusen | METHOD FOR DEGASSING LIQUIDS, AND DEVICE FOR CARRYING OUT THE METHOD |
US4382404A (en) * | 1981-06-23 | 1983-05-10 | Chemetron Process Equipment, Inc. | Vacuum screw loader |
JPS59155837A (en) * | 1983-02-24 | 1984-09-05 | Fuji Photo Film Co Ltd | Method for melting photographic material |
DE3332629A1 (en) * | 1983-09-09 | 1985-03-28 | Hermann Berstorff Maschinenbau Gmbh, 3000 Hannover | METHOD AND DEVICE FOR POWDERING POLYMERS |
-
1989
- 1989-12-26 FR FR8917515A patent/FR2656293B1/en not_active Expired - Fee Related
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1990
- 1990-12-07 JP JP3501295A patent/JPH05503031A/en active Pending
- 1990-12-07 WO PCT/FR1990/000890 patent/WO1991010164A1/en active IP Right Grant
- 1990-12-07 DE DE69006858T patent/DE69006858T2/en not_active Expired - Fee Related
- 1990-12-07 US US07/853,736 patent/US5264024A/en not_active Expired - Fee Related
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1991
- 1991-07-25 EP EP91900839A patent/EP0507795B1/en not_active Expired - Lifetime
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JPH05503031A (en) | 1993-05-27 |
FR2656293B1 (en) | 1992-06-12 |
FR2656293A1 (en) | 1991-06-28 |
DE69006858T2 (en) | 1994-09-08 |
DE69006858D1 (en) | 1994-03-31 |
WO1991010164A1 (en) | 1991-07-11 |
EP0507795A1 (en) | 1992-10-14 |
US5264024A (en) | 1993-11-23 |
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