JPS60193501A - High-pressure crystallizer - Google Patents

Abstract

PURPOSE:To improve the efficiency of removing liquid material in a high- pressure crystallizer and to prevent the deterioration of a filter as far as possible by improving the structure for attaching the filter. CONSTITUTION:An end ring 9 is fixed to the top end of a filter 2 and a cylindrical reinforcing member 10 is disposed via a heat insulating material 3 on the rear side of the filter 2. Said member 10 is mounted between the circumferential edge on the top surface of a feed and discharge side block 5 and the bottom surface of the ring 9 by adjusting the length thereof according to the axial length of the cylindrical filter 2 so that said ring 9 can be positioned. As a result the nearly the designed filtration function is provided and the component captured to high purity is obtd. at a high yield. Since the damage of the filter 2 is suppressed, the frequency of exchanging the filter is decreased.

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a high-pressure crystallizer, and particularly to a high-pressure crystallizer that improves the mounting structure of a filter, increases the removal efficiency of liquid substances, and prevents deterioration of the filter as much as possible. It is related to.

The high-pressure crystallization method involves introducing a raw material consisting of a liquid phase or slurry consisting of multiple components into a high-pressure container, and applying high pressure to the raw material with the liquid discharge pipe closed to crystallize specific components. This is a method of acceleration, and by this operation, a state is obtained in which crystals of a specific component (hereinafter sometimes referred to as a captured component) and residual liquid (hereinafter sometimes referred to as a removed component) are mixed.

Therefore, by unblocking the drain pipe, applying piston pressure to the solid-liquid coexistence state, and discharging the liquid removed component out of the system via the filter, and separating the solid-liquid without squeezing the remaining same phase, High purity specific components can be obtained. That is, FIG. 1 is a vertical cross-sectional view of the main parts illustrating an apparatus used for this type of high-pressure crystallization, in which 1 is a high-pressure vessel, 2 is a filter,
3 is the insulation material, 4 is the piston, 5 is the supply/discharge side block,
Reference numeral 6 indicates a raw material supply pipe, and 7 indicates a removed component discharge pipe.The following is a brief explanation of the basics of the high-pressure crystallization procedure using this apparatus.

(2) Close the liquid drain valve V and open the liquid supply valve v0 to supply the raw material from the raw material supply pipe line 6 into the high-pressure container 1;

(2) When the liquid supply is finished, the liquid supply valve V6 is closed, and the piston 4 is lowered to apply high pressure to the raw material in the container 1, thereby promoting crystallization of a specific component.

- When the crystallization is finished, open the drain valve V and move on to the filtration/squeezing process. In this step, the liquid present in the container 1 is squeezed and discharged through the filter 2, and the liquid passes through the gap provided on the back side of the filter 2, through the drain passage 8 of the supply/discharge side block 5, and into the discharge pipe. When the liquid reaches the waterway, it is discharged from the drain valve V.

(2) After filtration and squeezing are completed, the high-pressure container 1 is opened and the cake-shaped collected component is taken out under atmospheric pressure, or it is melted into a liquid and taken out from the high-pressure container.

By the way, in the above filtration/squeezing step (2), the filter is subjected to a high pressure differential action of several hundred to several thousand atmospheres.

Furthermore, the filter is affected by the frictional force associated with squeezing the solid, and is also affected by the internal pressure applied to the top surface of the upper end ring 2a and the differential pressure when the bottom surface of the ring 2a reaches atmospheric pressure (arrow ←) It is easy to compress and deform in the direction. In particular, in the case of a sintered metal (SUS, etc.) filter with a simple structure, the pores for liquid passage may be crushed by compressive deformation due to the above-mentioned stresses, and the filter function may be lost. It goes without saying that the cylindrical filter 2 is easily deformed in the direction of diameter expansion. Because of this, conventional high-pressure crystallizers
There were problems such as a decrease in the recovery rate due to local damage to the filter, or blockage of pores due to compressive deformation (resulting in a decrease in the purity of the collected material).

The inventors of the present invention have focused on these circumstances and have conducted various research efforts in an attempt to develop a mounting structure that can reliably prevent damage and compressive deformation of the filter. The present invention was completed as a result of such research, and its structure is to solidify and precipitate a specific component in a liquid phase mixture under pressure, separate the solid and liquid under pressure, and separate and recover the specific component. In a high-pressure J6-1 analyzer, at least the upper end of a cylindrical filter disposed on the inner circumferential wall of a high-pressure container is fixed to a ring, and the ring is prevented from deforming in the axial direction by a reinforcing member, and the inside of the high-pressure container is The gist is that the cylindrical filter is supported from the back side by the reinforcing member in addition to being placed at a predetermined position 61.

DESCRIPTION OF THE PREFERRED EMBODIMENTS The configuration and effects of the present invention will be explained in detail below with reference to the drawings. FIG. 2 is a schematic longitudinal cross-sectional view of a main part showing a filter attachment part of a high-pressure crystallizer according to the present invention, and the structure of the entire apparatus is substantially different from the example shown in FIG. 1. In this example, an end ring 9 is fixed to the upper end of the filter 2, and a cylindrical reinforcing member 1 is attached to the back side of the filter 2 via a heat insulating material 3.
0 is placed. The length of the reinforcing member 10 is adjusted according to the axial length of the cylindrical filter 2, and the reinforcing member 10 is installed between the upper peripheral edge of the supply/discharge side block 5 and the lower surface of the end ring 9. JI so that the ring 9 can be positioned.
J has been completed. Note that this reinforcing member 10 is provided with a heat insulating material 3 between it and the filter 2 (the insulating material 3 should be made of a material or structure that allows the liquid that has passed through the filter 2 to flow down in the direction of the discharged liquid passage gap 8 at the bottom). (Of course, it is natural that this is the case.) In the case of intervening a simple cylindrical one, it may be a simple cylindrical one.Alternatively, for convenience of attachment and detachment, it may be of a vertically split BS structure as shown in Fig. 3. If the heat insulating material 3 is not provided, a vertical slit (or vertical groove, etc.) 10a as shown in FIG. 4, for example, should be provided to allow the flow of the liquid that has passed through the filter 2. The size of this slit must be kept within a range that can achieve the purpose of reinforcement in the axial and radial directions. Furthermore, this reinforcing element 10 can also be formed integrally with the end ring 9.

By positioning the filter 2 with the end ring 9 and the reinforcing member 10 in this way and supporting it from the back side with the reinforcing member 10, the compressive force in the direction of the arrow (a) and the arrow ( ) Even if a diameter expanding force is applied in the direction, the filter 2
If the pores are deformed and damaged, there is a risk that the pores may become clogged or enlarged, and the PI overfunctions as expected, resulting in highly pure collected components being obtained at a high yield of 6. be able to. Moreover, since damage to the filter 2 is significantly suppressed, the frequency of its replacement can be extremely reduced.

FIG. 5 is a schematic longitudinal cross-sectional view of main parts showing another embodiment of the present invention, in which both the upper and lower ends of the filter 2 are connected to the end ring 9.
．． 9, and a reinforcing member 10 is attached between the end ring 9° and 9.
In this configuration, filter 2-
Since both ends of the ring are supported by the end rings 9°9, better stability is maintained against external forces in the compression direction and the expansion direction, and a reinforcing effect can be obtained.

FIG. 6 is a schematic vertical cross-sectional view of a main part showing still another embodiment of the present invention, which more effectively prevents damage to the filter, further increases filtration efficiency, and further improves the ease of attaching and detaching the filter 2, etc. It was designed so that it could be improved. That is, in this example, a cylindrical filter 2 having a taper that expands in two directions as it goes downward is used, and the heat insulating material 3 and reinforcing member 1
0 is similarly formed and installed between the end rings 9 and 90, and a spacer 1 having a wedge-shaped cross section is further provided on the outer periphery of these rings.
1 has bottomed out.

However, in order to prevent deformation of the filter 20 in the circumferential direction,
Although it is desirable to minimize the gap between the heat insulating material 3 and the reinforcing member 10 arranged on the back side of the filter 2,
As shown in FIGS. 2 and 5, the filter 2 and the reinforcing member 10
If the cylindrical parts are formed into the same diameter cylindrical shape without a taper, it is impossible to make the above-mentioned gap substantially zero when the ease of installation into the pressure-resistant container 1 is taken into account. However, if you have the configuration shown in FIG. 6, by bottom-fitting the wedge-shaped spacer 1i on the outer circumferential side of the tapered reinforcing member 10, the reinforcing member 10 can be pressed against the back side of the filter by the wedge effect. Since the gap can be reduced to substantially zero, the diameter expansion deformation of the filter 2 can be completely prevented. Furthermore, the filter 2 and the like can be easily removed by lowering the supply/discharge side block 5 and pushing down the filter 2 and the like from above. Also, during compression, a downward frictional force acts on the inner peripheral surface of the filter 2, but as shown schematically in FIG. Since the outer circumferential surface of the filter 2 receives a force in the direction t[L from the inner circumferential surface of the filter 2 due to the downward compressing force, there is less friction with the filter 2, and wear of the filter 2 is suppressed. At the same time, the squeezing force is easily transmitted to the lower end of the same phase. Furthermore, when the cake-like solid changes from the state shown by the pointed edge in Figure 7 to the state shown by the chain line, it is squeezed while repeating buckling failure, and at the time of this buckling failure, the liquid left inside Since a flow passage for substances is formed, the solid-liquid separation efficiency is also significantly improved.

In the above description, sintered metal was used as an example of the filter material, but any filter material may be selected. For example, single-layer or multi-layer wire mesh, perforated plates, or combinations of these with stacked sintered bodies, canvas, etc.
It can be arbitrarily selected depending on the pressure and the target material to be treated.

The present invention is configured as described above, and it has become possible to increase solid-liquid separation efficiency in high-pressure crystallization and to significantly suppress deterioration of the filter.

[Brief explanation of drawings]

FIG. 1 is a schematic vertical cross-sectional view illustrating a high-pressure crystallizer, and FIG.
Figure 5.6 is a schematic vertical sectional view of the main part illustrating the filter mounting structure of the high-pressure crystallizer according to the present invention, Figure 3.4M is a sketch diagram illustrating the reinforcing member used in the present invention, and Figure 7 FIG. 2 is an explanatory diagram showing a state of squeezing a cake-like solid. 1 Pressure-resistant container 2... Filter 3... Insulating material 5... Supply/discharge side block 10...
・Reinforcement member 11... Spacer application submitted Kobe Steel, Ltd.

Claims (1)

[Claims] A specific component in a liquid phase mixture is solidified and precipitated by applying pressure.
In a high-pressure crystallizer that separates solid and liquid under pressure to separate and recover specific components, at least the upper end of a cylindrical filter placed on the inner peripheral wall of a high-pressure container is fixed to a ring, and the ring is reinforced. A high-pressure crystallizer characterized in that the cylindrical filter is fixed at a predetermined position in the high-pressure container by a member, and the cylindrical filter is supported from the back side by the reinforcing member.