JPH0511297B2 - - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION [Industrial Application Field] The present invention relates to a method for gelling a photographic emulsion in which the photographic emulsion is dispersed in a pot-shaped container and gelled, and a gelling apparatus therefor.

[Prior Art] Conventionally, in the manufacturing process of photographic light-sensitive materials, photographic emulsions are prepared and then cooled to gel.The cooled photographic emulsions are stored in a gel state in a container and stored at low temperatures, and then coated on a support. When necessary, it is removed from the container and thawed again.

[Problems to be Solved by the Invention] A device for gelling such a photographic emulsion is one in which the photographic emulsion is divided into appropriate amounts, placed in a refrigerator, left, cooled from the outside by heat conduction, gelled, and stored. There is. Since the photographic emulsion is slowly cooled after being stored in a refrigerator, the photographic emulsion is exposed to undesirable high temperatures for a long period of time, and the necessary ripening progresses, resulting in deterioration of photographic performance such as fog. In addition, when silver halide grains have a large grain size, such as in an X-ray photographic emulsion, it takes time to set the grains, which may cause the grains to settle, resulting in uneven silver content distribution and fog.

Furthermore, as disclosed in Japanese Patent Publication No. 52-14717, a large number of thin-walled pipes are arranged side by side at intervals to allow cold and hot water to flow outside, and after putting photographic emulsion inside the thin-walled pipes, cold water is There is one that circulates, cools, and gels, and then circulates hot water to melt the gel, which then falls and is taken out. Since this uses heat conduction, it takes time to cool down. Furthermore, since it re-melts when taken out, the photographic emulsion adheres to the inner surface of the thin-walled pipe, resulting in contamination and poor cleaning performance.

Furthermore, as disclosed in Japanese Patent Publication No. 50-31447, the inside of a sealed container with a jacket and a heat transfer pipe for melting at the bottom is evacuated, the photographic emulsion is sprinkled and gelled, and cold water is directly poured into the jacket. There are some that are stored by circulating them, and when needed, can be taken out by pouring hot water through a heat transfer pipe and melting them. This is suitable for storing one large batch of photographic emulsions all at once, but storing a wide variety of photographic emulsions requires a large number of gelling devices, which requires a lot of space and cost. Not suitable for small quantity production.

Further, as disclosed in US Pat. No. 3,779,7551, after pre-boiling and cooling at a relatively high pressure in a passage with a predetermined degree of vacuum, the expansion tube is boiled again and cooled to gel in the device. And when taking it out from the device, it is heated with hot water to dissolve the gelled material around it. Since this is gelled in the expansion tube, there are problems in that when taking it out, the area around the gelled material has to be re-melted or cut, resulting in a lot of loss and poor cleaning performance.

This invention was made against the background of the above circumstances, and it not only improves the storage efficiency by directly storing the photographic emulsions in a pot-shaped container, but also makes it possible to miniaturize the device and to store a wide variety of photographic emulsions by gelling them. It is an object of the present invention to provide a method and a gelling device for emulsion gelling.

[Means for Solving the Problems] In order to solve the above problems, the invention of a method for gelling a photographic emulsion involves opening a conveyor shutter in a closed chamber, carrying an empty cup-shaped container into the closed chamber, The shutter is closed to seal the sealed chamber, and the degree of vacuum in the sealed chamber containing this cup-shaped container is adjusted to a pressure that makes the temperature near the sol-gel transition point the saturated vapor temperature. The photographic emulsion passes through the droplet growth tube, loses its latent heat of vaporization, and becomes instantaneously cooled droplets. The photographic emulsion is directly dropped into a cup-shaped container and gelled, stored as a gelled product in the cup-shaped container, and the conveyor shutter of the sealed chamber is opened to transport the cup-shaped container containing the gelled photographic emulsion from the sealed chamber. It is characterized by

In addition, the invention of the photographic emulsion gelling device is such that a transport shutter is provided in a closed chamber so that it can be opened and closed, and by opening and closing the transport shutter, a cup-shaped container can be taken in and out of the closed chamber. A vacuum generator is provided to adjust the temperature near the point to a pressure that makes it the saturated vapor temperature, and a supply liquid dispersion pipe is provided above the sealed chamber for dispersing the photographic emulsion as a supercooled sol onto the cup-shaped container. A liquid sprayer is provided at the tip of the supply liquid sprayer tube protruding into the sealed chamber, and a droplet growth tube opening downward is provided to cover the liquid sprayer, and the supercooled droplets of the photographic emulsion are dispersed. After spraying from above, the droplets are made to collide with each other in the droplet growth tube, and the scattering and agitation of the photographic emulsion towards the vacuum generator side is controlled to obtain a gelled product directly in the cup-shaped container. It is characterized by what it has done.

[Function] The invention of the photographic emulsion gelling method and its gelling device involves opening a conveyor shutter in a closed chamber, carrying an empty cup-shaped container into the closed chamber, and closing the conveyor shutter to seal the closed chamber. do. Then, the degree of vacuum in the sealed chamber housing this cup-shaped container is adjusted to a pressure that makes the temperature near the sol-gel transition point the saturated vapor temperature, and the photographic emulsion is supercooled from the top of the sealed chamber via the supply liquid distribution pipe. Spray as a sol onto a pot-shaped container. This photographic emulsion passes through a droplet growth tube, loses its latent heat of vaporization, becomes instantaneously cooled droplets, falls directly into a cup-shaped container, and gels.
It is stored as a gel in this pot-shaped container. This cup-shaped container is transported out of the sealed chamber with the gelled photographic emulsion contained therein by opening the transport shutter of the sealed chamber.

[Embodiment] An embodiment of the present invention will be described in detail below with reference to the accompanying drawings.

A conveyance roller 2 is disposed at the bottom of a sealed chamber 1 of a photographic emulsion gelling apparatus, and a conveyance shutter 3 is disposed at one side of this closed chamber 1. The container 4 is carried in and out of the closed room 1. The pot-shaped container 4 carried into the sealed chamber 1 is placed on the conveying roller 2.

Further, a vacuum generator 5 is provided on the upper side of the sealed chamber 1, and adjusts the inside of the sealed chamber 1 to a predetermined degree of vacuum. Furthermore, the upper part of the sealed chamber 1 is a supply liquid distribution pipe 6.
are connected in series, and a liquid sprayer 7 is provided at the tip of this supply liquid distribution pipe 6. Furthermore, the supply liquid distribution pipe 6
A droplet growth tube 8 is provided at the tip of the droplet growth tube 8 so as to cover the liquid sprayer 7.

The photographic emulsion 9 is supplied from the supply liquid dispersion pipe 6, and is dispersed into the closed chamber 1 by the liquid dispersion device 7, which causes it to boil, remove the latent heat of vaporization, and become instantaneously cooled droplets 10, resulting in droplet growth. It falls directly into the container 4 through the tube 8, gels, and is stored in the container 4 as a gelled product 11.

Next, the operation of this embodiment will be explained.

First, the transport shutter 3 is opened, and the empty cup-shaped container 4 is carried into the sealed chamber 1, placed on the transport rollers 2, and the transport shutter 3 is closed to seal it.

Next, the vacuum generator 5 is operated to bring the sealed chamber 1 to a predetermined degree of vacuum. Then, the photographic emulsion 9 is divided into required amounts using a known means such as a flow meter or a load cell, and is supplied to the supply liquid dispersion pipe 6 and sprayed into the sealed chamber 1 from the liquid dispersion device 7. This dispersion causes rapid boiling, removes the latent heat of vaporization, and instantly cools the water to a temperature that makes the pressure in the sealed chamber 1 the saturated water vapor pressure.

Photographic emulsion 9 normally transfers from sol to gel at around 20 to 25°C. This is called the sol-gel transition point, and if the pressure inside the sealed chamber 1 is maintained at 16 to 24 mmHg, the droplets 10 sprayed from the supply liquid spray pipe 6 are cooled to 20 to 25°C.

At this time, the temperature decreases instantaneously due to water evaporation, but there is a delay in the gelation of the sol, and the sol does not turn into a gel immediately but flows as a supercooled sol. The photographic emulsion 9 thus dispersed falls into the container 4 as cooled droplets 10 and maintains a fluid state, so that a uniform liquid level is formed in the cup-shaped container 4. After that, gelation progresses and the cup-shaped container 4
A gelled material 11 is obtained which is uniformly divided within the pores.
In order to divide the pot-shaped container 4 while maintaining a uniform surface in this way, it is preferable to maintain the pressure inside the sealed chamber 1 at a pressure that makes the temperature near the sol-gel transition point the saturated steam temperature.

Therefore, if the degree of vacuum in the sealed chamber 1 is adjusted to a pressure that makes the temperature near the sol-gel transition point the saturated vapor temperature, and the photographic emulsion 9 is sprayed from the supply liquid spray pipe 6 through the liquid sprayer 7, the spraying can be completed. The number of droplets 10 is 20~
Cooled to 25°C. The droplets 10 dispersed in this way fall into the cup-shaped container 4 as cooled droplets and maintain a fluid state, so that a uniform liquid surface is formed in the cup-shaped container 4 and the spraying point is There is no unevenness due to the formation of a protruding ridge with the apex directly below.

Further, the droplets 10 sprayed by the liquid sprayer 7 rapidly evaporate and cool down the moment they are sprayed, and then fall into the droplet growth tube 8. At this time, the droplets 10 collide with each other in the droplet growth tube 8 and grow, and most of them collide with the inner wall of the droplet growth tube 8 and flow down as a thin film. By appropriately selecting the aperture and length of the droplet growth tube 8, most of the droplets can be grown to a size that will not be mixed into the exhaust system 12 communicating with the vacuum generator 5.

Therefore, by having the droplet growth tube 8, even if rapid boiling occurs at the moment the droplets 10 are dispersed,
This prevents it from being mixed into the steam flow and being removed from the exhaust system 12 as a loss.

The supply pressure of the photographic emulsion 9 is preferably such that it prevents boiling before the liquid sprayer 7, and the temperature of the photographic emulsion 9 is preferably such that a pressure corresponding to the saturated water vapor pressure of water can be maintained. For example, when supplying at 40°C, it is desirable to maintain the pressure in front of the liquid sprayer 7 at 56 mmHg or higher. By maintaining this pressure, cooling within the supply dispersion pipe 6 can be prevented.

When the gelled material 11 is stored in the cup-shaped container 4, the transport shutter 3 is opened and the cup-shaped container 4 is taken out and stored in the refrigerator as it is.

The above operation can also be fully automated by known means. In addition, since the pot-shaped container 4 can be stored in a refrigerator equipped with a known automatic storage system, it is possible to take out the required amount when needed, making it suitable for high-mix, low-volume production and enabling quick processing. Become.

Further, the supply liquid distribution pipe 6, liquid distribution device 7, and droplet growth tube 8 can be washed by passing hot water or a cleaning chemical solution. Furthermore, the pot-shaped container 4 after use can be washed elsewhere by known means, and has good cleaning properties.

Furthermore, since the degree of vacuum inside the sealed chamber 1 is relatively low,
An inexpensive vacuum generator 5 can be used, for example a water ejector. Moreover, it is sufficient that the sealed chamber 1 can take in and out the cup-shaped container 4, and is compact and does not take up much space.

[Effects of the Invention] As described above, the present invention adjusts the degree of vacuum in the sealed chamber to a pressure that makes the temperature near the sol-gel transition point the saturated vapor temperature, and forms a cup-shaped photographic emulsion that can be taken in and out from the top of the sealed chamber. Sprayed into a container, this photographic emulsion is gelled using the latent heat of vaporization caused by boiling.
Gelation can be obtained by directly storing the photographic emulsion in the cup-shaped container, and the photographic emulsion quickly gels to improve its quality.Moreover, it can be stored in the cup-shaped container with a uniform surface, improving storage efficiency. .

In addition, since the photographic emulsion is directly gelled in a container that can be transported, it is possible to downsize the device.Moreover, this container can be transported in and out by opening the transportation shutter in the closed room, and can be transported in and out of the container. It is divided into containers of various shapes and is suitable for producing and storing a wide variety of products in small quantities.

In addition, the photographic emulsion to be scattered is guided by the droplet growth tube and falls while colliding with each other, and is mixed into the vapor stream at the moment of being scattered, so that the photographic emulsion is not scattered and mixed into the vacuum generator side. can be regulated, improving the durability of the device.

[Brief explanation of the drawing]

The drawing is a front view showing an embodiment of the present invention. DESCRIPTION OF SYMBOLS 1... Sealed chamber, 2... Conveyance roller, 3... Conveyance shutter, 4... Cup-shaped container, 5... Vacuum generator, 6... Supply liquid distribution pipe, 7... Liquid distribution device, 8
...Droplet growth tube.

Claims (1)

[Scope of Claims] 1. Open the transport shutter of the sealed chamber, carry the empty pop-up container into the sealed chamber, close the transport shutter to bring the sealed chamber into an airtight state, and transport the empty pop-up container into the sealed chamber containing the popped container. The degree of vacuum is adjusted to a pressure that brings the temperature near the sol-gel transition point to the saturated vapor temperature, and the photographic emulsion is sprayed as a supercooled sol from the upper part of the sealed chamber via the supply liquid spray pipe onto the cup-shaped container. This photographic emulsion passes through the droplet growth tube, loses its latent heat of vaporization, becomes instantaneously cooled droplets, falls directly into the cup-shaped container, and gels. A method for gelling a photographic emulsion, which comprises storing the gelled photographic emulsion in a cup-shaped container containing the gelled photographic emulsion by opening a conveyance shutter in the closed chamber and conveying the cup-shaped container containing the gelled photographic emulsion from the closed chamber. 2 A transport shutter is provided in the sealed chamber so that it can be opened and closed, and the cup-shaped container can be taken in and out of the sealed chamber by opening and closing the transport shutter, and the degree of vacuum in the sealed chamber is set to a pressure that makes the temperature near the transition point of the sol-gel the saturated vapor temperature. At the same time, a supply liquid dispersion pipe for dispersing the photographic emulsion as a supercooled sol onto the cup-shaped container is provided in the upper part of the sealed chamber, and a supply liquid dispersion pipe protruding into the sealed chamber is provided. A droplet growth tube is provided at the tip of the tube, and a droplet growth tube with an opening at the bottom is provided to cover the liquid distribution device, and after the supercooled droplets of the photographic emulsion are sprayed from above, the droplet growth tube is The photographic emulsion is characterized in that the droplets are made to collide with each other, and the scattering and agitation of the photographic emulsion toward the vacuum generator side is regulated to obtain a gelled product directly in the cup-shaped container. Gelling device.