JPH04145902A - Pressure crystallizer - Google Patents

Abstract

PURPOSE:To easily discharge a liq. phase by forming the liq. discharge means with a pressure waste soln. vessel connected to a high-pressure vessel through a discharge vessel, a mechanism for pressurizing the waste soln. in the vessel and a soln. discharge pipe connected to the waste soln. vessel through the soln. discharge valve. CONSTITUTION:A high-pressure vessel C, a means S for supplying a mixture into the vessel C, a means P for pressurizing the mixture in the vessel and a liq. discharge means F connected to the vessel C are provided. The liq. discharge means F is formed by a pressure waste soln. vessel 20 connected to the vessel C by a liq. discharge pipe 17 through liq. discharge valves V2 and V3, a mechanism 22 for pressurizing the waste soln. in the vessel 20 and liq. discharge pipes 18 and 19 connected to the vessel 20 through liq. discharge valves V1 and V4. Consequently, when pressure crystallization is carried out, a reduced-pressure nozzle is not clogged, a liq. phase is smoothly discharged, cavitation, erosion, etc., are prevented in the nozzle, and the liq. discharge rate is easily controlled.

Description

DETAILED DESCRIPTION OF THE INVENTION (Industrial Application Field) The present invention relates to a pressure crystallizer, and more specifically, a pressure crystallizer that solidifies a mixture of two or more components including a specific component by pressurizing it in a high-pressure container. The present invention relates to a pressure crystallizer applied to a pressure crystallization method in which a liquid phase is discharged outside a high-pressure container after a liquid coexistence state is established to form a solid product of a specific component.

(Prior art) Pressure crystallization has great potential for application to raw materials that are difficult to separate using conventional distillation and cooling crystallization methods, and it is easy to obtain high-purity products. It is a separation and purification technology that has been attracting a lot of attention as the chemical industry has become increasingly refined in recent years, due to its high yield, easy acquisition, and low energy consumption.

Such a pressure crystallization method and its apparatus are described, for example, in Chemical Industry 50.
Vol. (1986) p. 331 "Overview of pressure crystallization method and equipment"
It is described in. This will be explained below with reference to FIG. 3 (a diagram showing an overview of the process flow and apparatus).

The pressure crystallizer includes a high-pressure container C, a means S for supplying a mixture into the container C, a means P for pressurizing the heated mixture in the container C,
It mainly consists of a liquid discharge means F connected to the container C. This high-pressure container C is formed of a body fl+ and a lower lid (2), and the pressurizing means P is controlled by a hydraulic unit (3).
It consists of a piston (5) that moves up and down inside the piston (
5) and a crystallization chamber (4) is formed within the container (1). The mixture supply means S consists of a liquid supply valve (121), a raw material supply pump (8), and a pre-crystallization can (7) connected to the crystallization chamber (4) via a pipe αa.The liquid discharge means F is It consists of a pressure reducing mechanism (10) and a drain valve (11) which are connected to the crystallization chamber (4) by a pipe (9), and a drain tank (6) is connected to the drain valve (11) by a pipe. This pressure reduction mechanism (10) uses a pressure reduction nozzle with a minute diameter such as 0.10 to 0.45 mmφ.
4) A filter is arranged on the inner surface of the body (1).

Pressure crystallization is carried out as follows. First, the raw material is fed from the raw material tank (14) to the pre-crystallizer (7), cooled to generate seed crystals for pressure crystallization, and then transferred from the pipe αJ through the valve (12). The raw material is injected into the crystallization chamber (4). When the raw material fills in the crystallization chamber (4), the liquid begins to flow out through the overflow pipe (19) which has an opening at the tip of the piston, and this is detected. Valve (IZ, (II
), the piston (5) starts pressurizing the raw material. When the raw material is pressurized, crystallization of a specific substance in the raw material progresses, and the inside of the crystallization chamber (4) enters a solid-liquid equilibrium state under high pressure. The solid produced at this time is generally a substance of extremely high purity.

Continue to increase the pressure to a predetermined level. When this pressure is reached, a predetermined solid-liquid ratio (saturated state) is immediately reached, so the drain valve (11) is immediately opened and the piston continues to descend while maintaining this pressure. In this way, most of the solids pass through the filter on the inner surface of the body (1) without dissolving, and the liquid phase passes through the filter on the inner surface of the body (1).
The liquid is discharged to the drain tank (6) via the pressure reducing mechanism (10) and the valve (11) via the piping (9).

When the piston (5) continues to descend further, the crystallization chamber (4)
The group of crystal grains within is squeezed under pressure, and the remaining liquid between the crystal grains undergoes a so-called "squeezing action" and is discharged into the tank (6). When the piston (5) is subsequently lowered, the crystal grains are formed into one large lumpy solid product along the shape of the crystallization chamber (4). When the liquid is almost completely separated from the solid in this way, the drain tank (6
) The liquid phase pressure in the crystallization chamber (4), which is connected to will be done.

When the pressure of the liquid discharged from the crystallization chamber (4) drops to a predetermined pressure, the piston (5) stops descending and the piston (
5), and at the same time, the fuselage (1) is also raised.

Next, the solid product placed on the lower lid (2) is taken out by a take-out device (not shown), after which the body (1) is lowered and attached to the lower lid (2), and the raw materials are Return to the injection process and repeat the same process to continuously produce products.

(Problems to be Solved by the Invention) As described above, the conventional pressure crystallizer includes a high-pressure container C, a means S for supplying a mixture into the container C, and a mixture supplying the heated mixture in the container C. It is mainly composed of a pressurizing means P and a liquid discharging means F connected to the container C. Of these, the liquid discharging means F is composed of a pressure reducing mechanism 00) connected to the crystallization chamber (4) and a discharging means. The drain valve (11) is equipped with a drain tank (6).
) is connected to the pipe. This pressure reduction mechanism 00) uses a pressure reduction nozzle with a minute diameter as described above.

The purpose of using a vacuum nozzle with a micro diameter is to reduce the liquid phase discharge rate and further improve the product yield. That is, when the drainage rate is high, crystals tend to pass through the filter, resulting in a decrease in product yield. This is because when the drainage rate is reduced, the crystals adhere to the filter, and the adhesion layer further exerts a filter-like action, increasing the yield.

However, the pressure reduction nozzle with such a small diameter is used as the liquid discharge means F.
When used in
It is often the case that the hole in the pressure reducing nozzle becomes clogged and becomes clogged, making it impossible to discharge the liquid phase. Furthermore, since the flow velocity of the drained liquid at the hole of the pressure reducing nozzle is extremely high, cavitation and erosion may occur. Furthermore, since the outlet side of the decompression nozzle communicates with the drain tank under atmospheric pressure, the pressure difference between the inlet and outlet sides of the nozzle is extremely large, making it difficult to control the drain speed. There is.

The present invention has been made in view of these circumstances, and its purpose is to solve the above-mentioned problems of the conventional methods, and to solve the problems of the liquid phase due to pressure reduction nozzle blockage when performing pressure crystallization. A pressure crystallizer that can smoothly discharge the liquid phase without causing troubles such as stopping the discharge or causing cavitation/erosion at the vacuum nozzle, and also makes it easier to control the drainage speed. This is what we are trying to provide.

(Means for Solving the Problems) In order to achieve the above object, the present invention provides a pressure crystallizer having the following configuration.

That is, the pressure crystallizer according to the present invention includes a high-pressure container, a means for supplying a mixture into the container, a means for pressurizing the mixture in the container, and a liquid discharge means connected to the container. In the analysis apparatus, the liquid 4J discharge means or a pressure-resistant liquid drain container connected to the high pressure container by a liquid outflow pipe via a liquid outflow valve, a pressurizing mechanism for draining liquid in the waste liquid container, and This pressure crystallizer is characterized in that it is configured with a liquid discharge pipe connected to a liquid discharge container via a liquid discharge valve.

(Function) As explained above, the pressure crystallizer according to the present invention includes a liquid discharge means that is connected to a pressure-resistant liquid drain container connected to a high-pressure container through a liquid outflow pipe via a liquid outflow valve, and the liquid discharge means. It is configured to include a pressurizing mechanism for draining liquid in a liquid container, and a liquid discharge pipe connected to the liquid discharge container via a liquid discharge valve.

Using such equipment, pressure crystallization can be performed as described below. First, after injecting raw materials into a high-pressure container as in the case of the conventional apparatus described above, with the liquid discharge valve and liquid outflow valve closed, the mixture is brought to a predetermined pressure by pressurizing means as in the case of the conventional apparatus. Now boost the pressure.

Next, at the same time as opening the liquid outflow valve, the pressure inside the pressure-resistant liquid drain container is adjusted to a value slightly smaller than the pressure inside the high-pressure container using the pressure pumping mechanism for the drain liquid. The liquid phase is discharged through a liquid outflow valve and a liquid outflow pipe into the liquid drainage container at a required liquid drainage rate.

Subsequently, after closing the liquid outflow valve and opening the liquid discharge valve, the inside of the drainage container is pressurized by the drainage liquid pressurizing mechanism, and the liquid in the container is drained through the liquid discharge valve. Can be drained via tube. At this time, if a drain tank is connected to the drain pipe, the drain liquid will be discharged to the tank. Thereafter, the liquid phase is discharged from the high-pressure container by repeating the discharge of the liquid phase into the drainage container and the discharge from the drainage container.

Squeezing out of the remaining liquid after discharging the liquid phase can also be performed by the same method as for discharging the liquid phase. From this point on, products can be produced in the same manner as with conventional equipment.

As described above, according to the pressure crystallizer according to the present invention, the liquid phase in the high-pressure container can be discharged by the liquid discharge means configured as described above, and the liquid discharge means has a pressure reducing nozzle. Therefore, it is possible to stop liquid phase discharge due to pressure reduction nozzle blockage,
The liquid phase can be smoothly discharged without causing problems such as cavitation and erosion in the pressure reducing nozzle.

Further, when the liquid phase is discharged into the drainage container, the inside of the drainage container can be pressurized by the drainage liquid pressurizing mechanism, so that the difference between the liquid pressure in the high-pressure container and the liquid pressure in the drainage container can be reduced. Moreover, it is easy to adjust the hydraulic pressure difference. Therefore, the drainage rate can be more easily controlled.

In other words, the liquid discharge means according to the present invention is connected to a liquid outflow pipe from the high-pressure container as described above and a liquid discharge pipe to a drain tank or the like, and is equipped with a pressurizing mechanism for draining liquid. It is a pressure-resistant drainage container. It is preferable to provide at least two such drainage containers rather than one. If there is only one,
If it is not possible to discharge liquid into the drainage container and from the drainage container at the same time, or if there are two or more, one drainage container is used to drain the liquid from the other container at the same time. The container is capable of discharging jJF into the container, so that the liquid phase in the high-pressure container can be continuously discharged, and the discharge pattern can be discharged in a desired pattern.
Moreover, the drainage speed can be controlled more reliably.

(Examples) Example 1 The pressure crystallizer used in Example 1 is shown in FIG. 1, and an enlarged view of its liquid discharge means F is shown in FIG. 2.

This device is equipped with the following 9-hole liquid discharge means F and F2 in place of the piping (9), pressure reduction mechanism (10) and 1 NOV liquid valve (11) shown in Fig. 3 as the liquid discharge means F. It is ours,
Other points are the same as in FIG.

The liquid discharge means F1 is a liquid discharge pipe] I7) and (25)
The liquid outflow valve v2 and the pressure-resistant liquid drain container 12CI connected to the high-pressure container C, and the pressurizing mechanism (2
2), and a liquid discharge pipe (25) and (la) connected to the container 12G via a liquid discharge valve 1, and the limb pipe (18) is connected to the liquid drain tank (6). In addition,
The pipe (25) is a common part for liquid outflow and liquid discharge, and is used as a liquid outflow pipe or a liquid discharge pipe.

The pressure mechanism (22) includes a cylinder (23) connected to a hydraulic system (not shown), and a piston (21) that moves up and down inside the cylinder (23) using hydraulic pressure. (24) is a hydraulically acting part.

The liquid discharge means F2 is constructed in the same manner as the means F, and its surrounding portions are also constructed in the same manner. However, the liquid outflow valve is
3. The liquid discharge valve is indicated by v4, and the liquid discharge pipe is indicated by (19).

First, a mixture (solution) of raw materials is cooled in a pre-crystallizer (7) to generate seed crystals, and after being injected into the crystallization chamber (4), the liquid outflow valve V2. With V3 and liquid discharge valve Vv4 closed, the piston (5) was lowered by the pressurizing means P and pressurized to 1500 atmospheres.

Next, the liquid phase in the crystallization chamber (4) was discharged as follows. That is, after the above pressure is applied, immediately open the liquid outflow valve (2) of the liquid discharge means F, and while maintaining the pressure, the piston (5) is opened.
) and drain the liquid phase in the crystallization chamber (4) into the liquid outflow pipe (17).
and (25), the liquid is discharged to the drain container e2 (lI).

Subsequently, the liquid outflow valve v2 of the means F is closed, the liquid discharge valve v1 is opened, and the piston (
21) to pressurize the inside of the drain container +2[), and drain the drain liquid in the container 12Q to the drain tank (6) through the liquid drain pipe (25) and the decoy. Parallel to the liquid discharge means F2
Open the liquid outflow valve ■3 and connect the liquid outflow pipes (17) and (25).
The liquid is discharged to the drain container 2G.

Subsequently, the liquid draining means F+ drains the liquid container 3G as described above.
At the same time, the liquid outflow valve ■3 of the liquid discharge means F2
is closed, the liquid discharge valve v4 is opened, and the inside of the container C2G is pressurized by the pressurizing mechanism (22), and the container c! Drain the liquid inside O through the liquid drain pipe (
25) and (19) to drain into the drain tank (6).

Thereafter, the liquid drain container 12 [1
and subsequent discharge from said container (2(I)
In parallel with this, the liquid drain container 12 (
) and the subsequent discharge from the container were repeated to discharge the liquid phase from the crystallization chamber (4).

After the liquid phase was discharged, the remaining liquid was squeezed out and discharged. This discharge was carried out in the same manner as the liquid phase discharge described above. After draining the residual liquid, a solid product containing a specific component was taken out from the container. Thereafter, the process returned to the raw material injection process and the same process as above was repeated to continuously produce the product.

As a result, it was confirmed that the yield, purity, and other qualities of the product were the same as those obtained using a conventional pressure crystallizer. In addition, by using the liquid discharging means according to the present invention in place of the liquid discharging means in conventional devices, it is possible to solve problems in liquid phase discharge such as nozzle clogging in conventional devices, and also to solve new problems. It was confirmed that this was not a problem or a derivative.

(Effects of the Invention) According to the pressure crystallizer according to the present invention, when performing pressure crystallization, troubles such as stopping liquid phase discharge due to blockage of the pressure reduction nozzle and occurrence of cavitation and erosion in the pressure reduction nozzle occur. Therefore, the liquid phase can be discharged smoothly, and the drainage rate can be more easily controlled.

[Brief explanation of drawings]

FIG. 1 is a diagram showing an outline of a pressure crystallizer according to Example 1,
FIG. 2 is an enlarged view of the liquid discharge means portion of the apparatus, and FIG. 3 is a diagram showing an overview of a conventional pressure crystallizer and the pressure crystallization process flow. (1) - Pressure vessel (2) - Lower lid (3) - Hydraulic unit (4) - Crystallization chamber (5) - Piston
(6) - Drainage tank (7) - Pre-crystallizer (
8) - Raw material supply pump (91 (13-1 piping)
αω-Pressure reducing mechanism Gll (12 (161-1 valve)
04) - Raw material tank 051 - Overflow pipe
(1η-Liquid discharge pipe α81 (191-Liquid discharge pipe Q
Tow pressure-resistant drainage container (21) -- Piston (2
2) - Drainage pressure mechanism (23) - Cylinder (2
4) - Hydraulic working part (25) - Pipe C - High pressure container S - Mixture supply means P - Mixture pressurizing means F Liquid discharge means Liquid discharge means V2. V3 Liquid outflow valve ■1 ■4 Liquid discharge valve

Claims (1)

[Claims] (1) In a pressure crystallizer having a high-pressure container, a means for supplying a mixture into the container, a means for pressurizing the mixture in the container, and a liquid discharge means connected to the container, the liquid discharge means is , a pressure-resistant drainage container connected to the high-pressure container by a liquid outflow pipe via a liquid outflow valve, a pressurizing mechanism for draining liquid in the drainage container, and connected to the drainage container via a liquid discharge valve. A pressure crystallizer comprising: a liquid discharge pipe;