JP2563832Y2 - High pressure device - Google Patents

Description

[Detailed description of the invention]

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a high-pressure apparatus for directly observing a change in physical properties of a liquid or solid substance under a pressurized state.

[0002]

2. Description of the Related Art In a method of applying pressure to a liquid phase mixture containing two or more substances to solidify a specific substance in the mixture and then separating the solid and liquid, that is, a pressure crystallization separation technique generates pressure. It is important to know the relationship between the shape and size of the growing or growing crystal and the pressure in order to judge the ultimate separation and purification purity and yield. Furthermore, in the solid-liquid separation step of discharging the liquid phase from the mixture of the crystal and the liquid phase generated or grown by pressurization, it is possible to confirm that there is no outflow of crystals from the filter and observe the state of cake formation. Just as important. It is because obtaining these conditions experimentally is very useful, for example, for designing an actual plant.

[0003]

Conventionally, methods for detecting and observing the generation and growth of crystals include a method of measuring a volume change by a fluid pressure cylinder device and a method of generating crystals inside a high-pressure container having an optical window. There is a method of visually observing the situation. However, in the former method of measuring a volume change, the crystal cannot be directly observed, and it is impossible to know the influence on the separation accuracy and the yield by the crystal shape and the like. The latter method of visual observation, for example, the method using an optical cell, can observe the state of the crystal inside, but because it is not a structure that can be pressed,
No separation and squeezing conditions can be observed.

[0004] In the latter case, as a countermeasure, it is conceivable to provide a piston closely fitted to the inner diameter of the optical cell, which makes it possible to squeeze and easily observe the state of separation and squeezing. However, the optical cell cannot increase the size of the window. For example, when observing a pressure state of 2000 kgf / cm ² , the size of the window should not be larger than 20 mm due to the strength of the material (sapphire, glass). Difficult,
With this size, it is possible to observe only the state of separation and squeezing in a limited range directly facing the window with a narrow field of view, and to observe the generation and growth of crystals that occur in a wide range in the optical cell from a wide angle It is impossible to do.

[0005] The pressure crystallization separation technique has been described above as an example of a liquid substance. However, the present invention is not limited to this. For example, a solute component is precipitated from a fluid in which a solute is dissolved, solid-liquid separation is performed, and a precipitate is recovered. As in the case of the above, the point that a change in physical properties of the solid substance under a pressurized state can be observed only in a narrow range is the same as in the above-described case.

The present invention has been made in order to solve such a problem, and an object of the present invention is to provide a general overview of all the situations of separation and squeezing under high pressure.
It is an object of the present invention to provide a novel device that can be easily visually observed under a wide field of view by an optical window having a small diameter and a pressure-resistant structure.

[0007]

The present invention has the following configuration to achieve the above object. That is, the present invention provides a pressure vessel having an optical window made of a hard transparent body and containing a transparent pressure-medium fluid, and a transparent vessel of a piston-type cylinder whose peripheral wall is housed in the pressure vessel and made of a transparent body. A first pressure mechanism extending from the transparent container, connected to a slidably protruding piston rod outside the pressure container via a sealing material, and pressurizing a fluid to be pressurized in the transparent container; A second pressurizing mechanism for pressurizing the transparent pressure-medium fluid within the same or substantially the same pressure as the pressurized fluid;
A liquid discharge line capable of separating a liquid component from the fluid to be pressurized in the transparent container and discharging the separated liquid to the outside of the pressure vessel, wherein the inside of the transparent container in a high-pressure state can be externally observed through the optical window of the pressure vessel. A high-pressure device characterized by the following.

In the present invention, the transparent container is made of sapphire,
It is a high-pressure device whose preferred embodiment is made of glass or a polymer material.

Further, the present invention is a high-pressure apparatus in which the optical window is preferably formed by a light receiving end member of an optical fiber.

[0010]

According to the present invention having the above-described structure, the fluid to be pressurized is supplied into the transparent container, and the fluid to be pressurized is pressurized by the first pressurizing mechanism. At the same time, the second pressurizing mechanism is also operated to increase the pressure inside and outside so that no pressure difference occurs. It is possible to observe, from the optical window of the pressure vessel, a state in which, for example, crystals are generated from the fluid to be pressurized in response to the pressurization and grow by the further pressurization.

Next, the liquid discharge line is operated to separate the liquid component in the fluid to be pressurized and discharge it to the outside of the pressure vessel. At this time, a situation in which crystals are formed in a cake shape can be observed from the optical window.

In this case, since the optical window provided in the pressure vessel is spaced apart from the transparent container at a considerable distance, almost the entire transparent container is positioned within a range that can be seen through the optical window. It is easy to compose, so even if it is an optical window with the same diameter of 20 mm as the conventional one, all of the changes in physical properties under high pressure in the transparent container are generally small, The window allows easy visual observation under a wide field of view.

Further, according to the present invention, the state of pressurization between the first pressurizing mechanism and the second pressurizing mechanism is controlled so that a pressure difference between the inside and outside is not always generated or a slight pressure difference is generated. Thus, the transparent container will not be destroyed. In addition, it is possible to provide a plurality of optical windows in a dispersed manner,
Applicable to equipment with large processing volume.

[0014]

FIG. 1 is a schematic structural view showing an embodiment of the present invention. The pressure vessel 1 includes a cylinder main body 1A, an upper lid 1B, and a lower lid 1C. Two frusto-conical holes are provided on the peripheral wall of the cylinder main body 1A so as to face each other such that the inner surface side has a large-diameter portion and the outer surface side has a small-diameter portion. Optical windows 2 are fitted in a liquid-tight manner. The optical window 2 is formed of sapphire, glass, or a polymer material, and cannot have a large size depending on pressure due to its strength. For example, when the pressure is 2000 kgf / cm ² , the diameter is limited to about 20 mm.

A transparent container 3 is provided inside the pressure container 1. The transparent container 3 is formed as a piston-type cylinder having a transparent peripheral wall made of sapphire, glass, or a polymer material. A piston rod 4 is fitted in the transparent container 3 in a sealed state, and can pressurize a fluid 16 to be housed therein. The lower part of the transparent container 3 is fitted to the lower lid 1C of the pressure vessel 1 in a sealed state, and the lower lid 1C
, A discharge passage 5 communicating with the inside of the transparent container 3 is provided therethrough. A filter 6 is disposed at an inner end of the discharge passage 5 in the lower lid 1C, and the filter 6 and the discharge passage 5 separate a liquid component from the pressurized fluid 16 in the transparent container 3. Thus, a liquid discharge line that can be discharged to the outside of the pressure vessel 1 is configured. On the other hand, a liquid supply passage 7 penetrates through the piston rod 4 at both upper and lower ends, and an on-off valve
It is connected to a liquid supply pipe having 14. The piston rod 4
It penetrates through a hole provided in the upper lid 1B of the pressure vessel 1 via a pressure sealing material and is slidably projected to the outside, and is connected to a first pressurizing mechanism 8 composed of, for example, a hydraulic press device. The pressure line of the first pressure mechanism 8 is provided with a pressure gauge 9, an automatic pressure regulating valve 12, and the like.

In the space around the transparent container 3 in the pressure container 1,
A transparent pressure medium fluid 17 such as water, alcohol, or the like is filled, and the surrounding space communicates with the outside via a pipe and is connected to the second pressurizing mechanism 10. The pressure line of the second pressure mechanism 10 is provided with a pressure gauge 11, an automatic pressure regulating valve 13, and the like.

The high-pressure device having the above-described structure includes a pressure gauge 9 for indicating an oil pressure (a fixed ratio) corresponding to the inside of the transparent container 3.
And the value of the pressure gauge 11 indicating the pressure around the transparent container 3 so that there is no difference, or even if there is, the oil pressure of the first pressurizing mechanism 8 The liquid pressure of the transparent pressure medium fluid 17 is controlled. Therefore, if one of them rises too much, the automatic pressure regulating valves 12 and
13 releases the pressurized fluid. Conversely, if the pressure drops too much, pressurization is advanced. These are automatically operated and controlled so that the pressure difference between the inside and outside of the transparent container 3 becomes almost zero.
Therefore, the transparent container 3 made of sapphire or glass is
Since it is the same pressure inside and outside, there is no destruction at all.

The operation of the above device is as follows. The pressurized fluid 16 to be pressurized is supplied into the transparent container 3 through the liquid supply pipe and the liquid supply passage 7, the on-off valve 14 is closed, and the first pressurizing mechanism 8 controls the pressure in the transparent container 3. The pressurized fluid 16 is pressurized. At the same time, the second pressurizing mechanism 10 is also operated to increase the pressure inside and outside so that no pressure difference occurs. Crystals are generated from the fluid 16 to be pressurized in response to the pressure increase, and the state in which the crystals grow by the further pressurization can be observed from the optical window 2 of the pressure vessel 1.

Next, the on-off valve 15 is gradually opened to operate the liquid discharge line, and the liquid in the pressurized fluid 16 is separated by the filter 6 and discharged to the outside of the pressure vessel 1. In the process, a situation where crystals are formed in a cake shape can be observed from the optical window 2. In the meantime, the pressurized state between the first pressurizing mechanism 8 and the second pressurizing mechanism 10 is controlled so that a pressure difference between the inside and outside is not always generated. When the cake begins to form, the pressure of the discharged liquid gradually decreases, but the force from the first pressurizing mechanism 8 is the sum of this liquid pressure and the pressure supported by the solid (cake), and this value is the initial value. The pressure is the same as that when only the liquid is used, the pressure difference between the inside and outside of the transparent container 3 does not differ, and the transparent container 3 does not break.

When the separation and the squeezing are completed, the first pressurizing mechanism 8 and the second pressurizing mechanism 10 are simultaneously operated so that there is no difference between the oil pressure applied to the piston rod 4 and the pressure of the transparent pressurized fluid 17 in the pressure vessel 1. The pressing force of After releasing the pressure, the liquid in the pressure vessel 1 is discharged, and the upper lid 1B and the lower lid 1C are opened to take out the transparent container 3. Thus, a series of operations is completed.

Conventionally, for example, when separating fats and oils,
Usually, crystals of fats and oils are fine and soft, so pressing with strong force in this state causes clogging of the filter, which makes it impossible to discharge the liquid inside, so that the purity cannot be increased, and because the crystals are soft, During the squeezing, it ran out of the filter and the yield was poor. Even in the case of such separation, if the apparatus according to the present invention is used, it is confirmed by visual observation that the crystals have grown sufficiently, and the separation is performed by squeezing to such an extent that no outflow occurs from the filter by adjusting the pressure. The rate can be secured and the purity can be increased.

In the above embodiment, since the optical window 2 has a truncated conical shape, the viewing angle can be made wider than that of a cylindrical shape having the same diameter, and the optical window 2 has a wedge shape. Therefore, it is also excellent in pressure resistance. In addition, as the optical window 2,
It is not limited to such a truncated cone shape, and a columnar shape or the like can be used, and is included in the scope of the present invention. In the case of using a cylindrical optical window, for example, by providing a cylindrical optical window 2 as shown in FIG. 2 or 3, pressure resistance and liquid tightness can be secured.

Although the embodiment uses the optical window 2 made of a transparent material such as sapphire or glass, it is also preferable to use a light receiving end member for an optical fiber. Observation is possible at a position remote from the first, and such a modification is also included in the scope of the present invention.

[0024]

As described above, according to the high-pressure apparatus according to the present invention, it is possible to visually observe the crystal growth process (crystal shape and size), the separation state, and the compression state from the generation of the crystal under high pressure. , Attained purity and yield can be accurately determined. In this case, the optical window 2 provided in the pressure vessel 1 can be arranged at a distance from the transparent container 3 in which the fluid to be pressurized is stored. Observation in a wide field of view is possible. Further, since the pressure can be adjusted in a state where the pressure difference between the inside and outside of the transparent container 3 is eliminated by adjusting the pressure between the first pressurizing mechanism 8 and the second pressurizing mechanism 10, there is no danger of the container being damaged and the reliability is improved. high,
Further, there is an advantage that the pressure processing volume can be increased.

[Brief description of the drawings]

FIG. 1 is a schematic structural view of a high-pressure device according to an embodiment of the present invention.

FIG. 2 is a diagram illustrating an outline of an example of a method of fitting an optical window in the high-pressure device according to the present invention.

FIG. 3 is a diagram showing an outline of an example of a method of fitting an optical window in the high-voltage device according to the present invention.

[Explanation of symbols]

1-Pressure vessel 2-Optical window
3-transparent container 4-piston rod 5, 6-liquid discharge line
7—Liquid supply passage 8—First pressurizing mechanism (hydraulic press device) 10—Second
Pressurizing mechanism (pressurizing device) 16--Pressurized fluid 17--Transparent pressurized fluid.

Claims (3)

(57) [Scope of request for utility model registration] 1. A pressure vessel having an optical window made of a hard transparent body and containing a transparent pressurized fluid, a transparent vessel of a piston type cylinder whose peripheral wall is housed in the pressure vessel and made of a transparent body, A first pressurizing mechanism that extends from the transparent container and that is connected to a piston rod slidably protruding through a sealing material to the outside of the pressure container and pressurizes a fluid to be pressurized in the transparent container; A second pressurizing mechanism for pressurizing the transparent pressurized fluid to the same pressure or substantially the same pressure as the pressurized fluid,
A liquid discharge line capable of separating a liquid component from the fluid to be pressurized in the transparent container and discharging the separated liquid to the outside of the pressure vessel, wherein the inside of the transparent container in a high-pressure state can be externally observed through the optical window of the pressure vessel. A high-pressure device characterized by the following. 2. The high-pressure device according to claim 1, wherein the transparent container is made of sapphire, glass, or a polymer material. 3. The high-pressure device according to claim 1, wherein the optical window is formed of a light receiving end member of an optical fiber.