JPS62191035A - Pressure-crystallizing apparatus - Google Patents

Abstract

PURPOSE:To simplify a seal structure and to prevent the generation of shearing force in a filter, by providing an elastic pressurizing partition wall separating a pressure medium and a material to be crystallized and providing the filter in the side of the material to be crystallized so as to leave an almost equal distance from the elastic pressurizing partition wall. CONSTITUTION:A material 26 to be crystallized is quantitatively supplied into a receiving bag 8 through a filter 13 and a pressure medium such as hydraulic oil is supplied between a container 2 and an almost cylindrical pressurizing partition wall 7 under pressure through a pressure port 2a. Subsequently, the material to be crystallized is pressurized under required high pressure through the partition wall 7 and the bag 8 to precipitate a crystal. Thereafter, only a liquid is discharged through the filter 13 and a drain pipe 8. By this constitution, a sliding ultrahigh pressure seal structure as is conventional is not required at all and, further, it is unnecessary to apply a corrosion resistant liner to the inner surface of the pressure container 2 because the pressure container is not directly contacted with the material to be crystallized. Furthermore, because no relative motion or shearing force is generated between the crystal and the filter, smooth and homogenous crystallization can be expected.

Description

DETAILED DESCRIPTION OF THE INVENTION (Industrial Application Field) The present invention relates to an improvement in a pressure crystallizer that precipitates crystals by pressurizing a material to be crystallized under ultra-high pressure.

(Prior Art) It is known that the material to be crystallized is pressurized under ultra-high pressure to precipitate crystals of a liquid, and as shown in Fig. 10, the material to be crystallized is placed in a container. Means is used to house the container and pressurize it with a piston. That is, in the same figure, a piston 24 of a hydraulic cylinder 23 provided on the press frame 21 side is inserted into a processing container 22 installed in a press frame 21 as a pressurizing member so as to be able to move up and down. The crystallization material 26 is supplied in a constant quantity into the processing container 22 via the supply pipe line 27, and the piston 24 descends via the hydraulic pipe line 28, and the material to be crystallized 26 is fed into the processing container 22, for example, by
The crystals are precipitated by applying pressure under ultra-high pressure of approximately kgf/cffl, only the waste liquid of the material to be crystallized is discharged from the drain pipe 30, and the replacement gas is sent into the container 22 through the gas replacement pipe 29. This allows, for example, recovering P from a P-lynchresol solution. The device shown in Fig. 10 is a pilot device to demonstrate the possibility of adiabatic pressure crystallization, and is intended to recover P from P-rich cresol at a pressure of 2000 K.
gf/am! , capacity 1.51, raw material injection temperature 10-50
℃, pressurization speed 10sec/2000kgf/c+J, cycle time 2m1n (minimum), P
-Results using feedstock with a concentration of 30χ indicate a cycle time of 3
With a purity of about m1n, the achieved purity was 99.5χ, and the recovery rate was close to the calculated value of 90χ. The one illustrated in FIG. 9 shows one example of such a pressure crystallizer that is in practical use industrially. The material to be crystallized 26 is supplied through the supply path 4a into the filter 13 which is provided upright between the upper lid 3 and the lower M4 and with a heat insulating layer 14 formed by a space between the inner surface of the container 2 and the piston. 15, and the drained liquid is filtered by the filter 13, and the liquid is drained from the drain path 6a provided at the outer lower M (packing gland) 6 of the four lower lids and communicating with the lower end of the cross-sectional layer 14. It is discharged. The means for supplying the pressure medium for pressurization and the material to be crystallized 26 shown in FIG. 10 are also used in FIG.

(Problem to be solved by the invention) The problems with the above-mentioned conventional technology are as follows.

Since this is a type in which a piston is pushed directly into the pressure vessel to apply pressure, a sliding ultra-high pressure seal is required for the material to be crystallized itself, and depending on the liquid properties of the material, measures such as applying a corrosion-resistant liner to the inside of the vessel may be required. Not only that, but the crystals move relative to the filter, generating shearing force on the filter, and in the final stage of crystallization it becomes similar to powder, resulting in pressure distribution and uneven squeezing. A problem arises.

(Means for Solving the Problems) In order to solve the above-mentioned problems, the present invention completely partitions the material to be crystallized and the pressure medium by an elastane partition wall, and has a sliding seal structure like the conventional type. In addition, the filter structure has been improved so that the pressure applied to the crystallization reservoir is uniform and perpendicular to the filter, so that the pressure is equalized during the compression stage. Specifically, in a pressure vessel equipped with a supply means for a pressure medium and a supply means for a material to be crystallized, an elastic pressure partition is provided to separate the pressure medium and the material to be crystallized. , a filter is provided on the side of the material to be crystallized at substantially the same distance below the elastic pressure corner wall.

(Function) According to the technical means of the present invention, as shown in FIG. 1, although the illustrated example shows a pressure crystallizer using cold isostatic pressing means (CIP method), 1 to receive the axial force of the pressure vessel 2, and upper and lower M
3 and lower lid 4 are each outer lower M (packing land)
5 and an outer lower lid (banking land) 6, and extends between the outer lower lid 5 and the outer lower lid 6, and is spaced from the inner surface of the container 2 and has a substantially cylindrical shape that forms an elastic pressurizing partition. A pressurized rubber mold 7 is disposed in a sealed manner, and a pressurized capo 2a is provided in the container 2 to communicate with the gap, so that the material to be crystallized extends between the lower end of the upper lid 3 and the upper end of the lower lid 4. A material storage bag 8 is also interposed in a sealed manner, and both upper and lower ends of the bag 8 are attached to the upper lid 3.
, are fixed to the lower lid 4 side, a supply/discharge passage 16 for the material to be crystallized is provided on the lower lid 4 side, and a filter 13 is provided at the open end of the supply/discharge passage 16 that communicates with the storage hang 8 side. A supply pipe line 17 from the tank 9 side of the first material to be analyzed 26 is communicated with one end of this supply/discharge passage 16 via a shutoff valve 10 .
Drainage pipe 1 equipped with shutoff valves 11a and llb at the other end
B, and by providing a gas supply path 19 on the upper M3 side in communication with the storage hang 8, and by communicating a gas replacement pipe 20 with the gas supply path 19 via the shutoff valve 12, the following can be achieved. Crystallization can be carried out using A fixed amount of the material to be crystallized 26 is supplied from the tank 9 through the shutoff valve 10, the supply/discharge path 16, and the filter 13 into the storage bag 8. After closing the shutoff valves 10, 11, and 12 sides, the pressure capacitor −
) 2a, a pressure medium (pressure oil, etc.) is fed between the container 2 and the pressurized rubber mold 7, and the material to be crystallized 26 is fed through the rubber mold 7 storage bag 8 under the required ultra-high pressure. After that, the shutoff valve 11 side is opened, the shutoff valve 12 is opened, and the displacement gas is sent from the displacement pipe 20 to the gas supply passage 19 into the storage bag 8 to remove the material to be crystallized. Only the liquid is discharged from the drain pipe 18 via the filter 13, the supply/drain passage 16, and the shutoff valve 11 side. According to this, the material to be crystallized 26 and the pressure medium are completely separated by the pressure gum mold 7, which is an elastic pressure partition wall, and further by the storage bag 8.
In order to pressurize the material 26 to be crystallized, even if a seal structure is provided, it is a fixed seal structure, and there is no need for a sliding ultra-high pressure seal structure. Furthermore, there is no risk that the material to be crystallized 26 will come into direct contact with the pressure vessel 2. Furthermore, since the pressure is applied in the same direction, the force is always applied to the filter 13 in the perpendicular direction, and the pressure is even during the squeezing stage, and the crystals move relative to the filter, causing shearing force to be applied to the filter 13. There is no longer any possibility of this occurring.

(Example) Each example of the apparatus of the present invention will be sequentially explained with reference to FIG. 2 and subsequent figures.

The embodiment shown in FIG. 2 is an embodiment in which the pressurizing rubber mold 7 as an elastic pressurizing bulkhead and the storage bag 8 in the embodiment shown in FIG. The structure shown is a pressure rubber type/crystallization material storage bag 7a, and in this embodiment, the gas exchange means is omitted and the pressure boat 2a is provided on the upper lid 3 side. This allows the lower outer M5 and lower outer lid 6 shown in the example in Figure 1 to be absorbed into the upper M3 and lower lid 4 sides, and in this case, the above-mentioned pressurized rubber type and crystallization target material are used. The storage hook 7a is shaped like a tubular bag, and one end of the opening of the tubular bag is fixed to the lower lid 4 side. Since the other parts are the same as those shown in FIG. 1, the parts below tank 9 are omitted.

The embodiment shown in FIG. 3 uses a pressurized rubber mold 7 in the shape of a bag cylinder and a storage bag 8, and supports the open lower end of the pressurized rubber mold 70 on the outer lower lid 6 on the lower M4 side. , tubular storage bag 8
The lower end of the opening is supported on the lower M4 side, and the gas replacement means is omitted as in the embodiment shown in FIG.
2a is provided on the upper M3 side. These second
．． In the embodiment shown in Fig. 3, the pressurizing elastic partition walls 7 and 8 are shaped like bag tubes, so that pressurization is performed from three directions, thereby reducing distortion on the corner wall side and uniformly distributing the object to be processed. It is advantageous in terms of compression. In addition, when such a gas replacement means is omitted, the liquid discharge of the material to be crystallized after crystallization is performed by pressurizing the pressure medium at a low pressure.

In the embodiments of FIGS. 1 to 3, the filter 1
3 was placed at the upper end of the lower M4 at approximately the same distance below the elastic pressurizing partition wall.However, as for the installation structure of the filter, the structure shown in each embodiment shown in FIG. 4 and subsequent figures can be adopted.

In the embodiment shown in FIG. 4, the pressurized rubber mold 7 and the storage bag 8 are the same as those shown in the embodiment in FIG. As shown in the figure, a cylindrical filter 13 is vertically installed vertically across the center of the upper lid 3 and the lower M4, and therefore a supply path 16a and a discharge path 16b for the material to be crystallized 26 are provided. are separated and provided at different locations as shown. Therefore, when it comes to draining liquid after pressure crystallization, the drain path 1
The pressure on the 6b side is gradually reduced, and the waste liquid is discharged through the filter 13. According to this filter 13, the filter 13 receives only compression, and when a porous or mesh filter is used as the filter material,
This is advantageous in terms of strength, and the filter filtration area can be significantly increased compared to the embodiments shown in FIGS. 1 to 3.

In the embodiment shown in FIG. 5, the cylindrical filter 13 in the embodiment in FIG. There will be increased benefits and compactness.

The embodiment shown in FIG. 6 uses the bag-tube-shaped pressurized rubber mold 7 and the storage hook 8, which were previously explained in the embodiment of FIG. According to this, as in the embodiment of FIG. 3, the strain on the elastic pressurized corner wall side is reduced by applying pressure from three directions, and the material 26 to be crystallized is compressed in the same direction. It's advantageous.

In supplying and discharging the material to be crystallized 26, it is divided into a supply path 16a and a discharge path 16b, similar to the embodiment shown in FIG.

The embodiments shown in FIGS. 7 and 8 are similar to those shown in FIGS.
In each of the embodiments shown in the figures, the pressurized rubber molds 7 are all installed on the side of the container 2, whereas the pressurized rubber molds 7 are each shaped like a bag cylinder, and the upper end of the opening is placed on the upper M3 side. The pressure rubber mold 5 is supported by a pressure bar 2a, and a filter 13 is disposed on the outside surrounding the pressure rubber mold 5, extending over the upper and lower lids 3.4. In this case, the filter 13 of the embodiment shown in FIG. 7 is cylindrical, whereas the embodiment of FIG. 8 differs in that the filter 13 is shaped like a bag cylinder. As shown by the supply path 16a, the material to be crystallized 26 is fed to the filter 13.
and the pressurized rubber mold 7, and the drained liquid is discharged through the discharge path 16b.
As shown in FIG. 2, this is carried out through a heat insulating layer 14 formed by the space between the filter 13 and the inner surface of the container 2.

According to this, the storage bag 8 can be omitted, and the filtration area of the filter 13 can be significantly increased.

It goes without saying that in the embodiments shown in FIGS. 1 to 6, the pressurized rubber mold 7 and the pressure medium between the rubber mold 7 and the inner surface of the container function as a heat insulating layer.

(Effects of the Invention) According to the present invention, the material to be crystallized and the pressure medium are separated by the elastic pressurizing partitions 7 and 8 in all embodiments, compared to the conventional pressure crystallizer of the piston-push type. ζ completely separated,
As a result, there is no need to use a sliding ultra-high pressure seal structure in the required parts as in the past, and all seal structures can be made into a simple fixed seal structure with no risk of leakage. The structure is simplified, and by arranging the filter almost equidistantly below the elastic pressure partition, the filter area can be easily increased and the filtration area can be increased.
It improves efficiency, eliminates the relative movement between the crystal and the filter and the generation of shearing force, and in combination with equal pressure, achieves uniform pressure during the compression stage, ensuring smooth and homogeneous crystallization. It can be done.

[Brief explanation of drawings]

FIG. 1 is a longitudinal sectional front view of an embodiment of the apparatus of the present invention, FIGS. 2 to 8 are longitudinal sectional front views of each main part of a modified embodiment of the same apparatus, and FIG. 9 is a longitudinal sectional view of an example of a piston-type crystallizer. The front view and FIG. 10 are explanatory diagrams of the basic structure of the pressure crystallizer. 1...Press frame, 2-Pressure vessel, 3-Top lid, 4
・-・Lower lid, 7・-・Pressure rubber type (pressurized elastic partition), 8
- Storage bathoge, 26. - Material to be crystallized. Figure 6 Figure 70 J7rA toa 4 16b

Claims (1)

[Claims] 1. An elastic pressure partition separating the pressure medium and the material to be crystallized is provided in a pressure vessel equipped with a supply means for a pressure medium and a supply means for a material to be crystallized, and the elastic pressure partition A pressure crystallizer characterized in that a filter is provided on the side of the material to be crystallized at approximately the same distance below.