JPH0463103A - Pressure crystallizer - Google Patents

Abstract

PURPOSE:To drastically improve productivity by providing a passage communicating with a raw slurry chamber and a separative compression chamber and a valve for opening and closing the passage to a piston. CONSTITUTION:A raw material is introduced into a raw material tank, a solid outlet 20 is closed by a valve rod 15, a piston 12 is positioned at the lowermost part of a vessel 10, and the raw slurry is supplied into a raw slurry chamber 14 by a high-pressure pump 16. An automatic valve V6 is then opened to communicate a liq. discharge pipe 18 with a liq. discharge pipe 6, a valve V3 of the passage 19 in the piston is opened, the piston 12 is raised to the center of the vessel 10, and half of the raw slurry in the chamber 14 is injected into a separative compression chamber 13 through the passage 19. The valve V3 of the passage 19 is closed, the piston 12 is lowered to press the raw slurry in the chamber 13 to 1500 atm, and a crystal is deposited. The valve V4 of the pipe 6 is opened to discharge the liq. into a tank T1, and a solid is formed in the chamber 13.

Description

[Detailed description of the invention] (Industrial application field) The present invention relates to a pressure crystallizer.

(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.

A typical example of a conventional apparatus used in such a pressure crystallization method is shown in FIG. In Figure 2, (9) is a pressure vessel;
(1) is a pressure-resistant cylinder constituting the container (9), (2) is a cylindrical filter for solid-liquid separation disposed on the inner peripheral wall of the cylinder full, and (3) is a cylinder (1). ), (4) is a pressurizing/squeezing piston that is fitted from the upper opening of cylinder (1), (5) is a raw material supply pipe, and vl is a supply pipe. A liquid valve, (6) is a drain pipe, v2 is a drain valve, +71 is a button for solid phase separation pressure, and (8) is a soyute for solid phase separation.

Regarding the procedure for performing pressure crystallization using the above equipment,
Representative examples thereof will be explained below.

fat Drain valve v2 is closed, and liquid supply valve 1 is opened to supply the raw material from the raw material supply pipe (5) into the container (9).

The raw material is a mixture of two or more components containing a specific component, and usually contains seed crystals of the specific component to promote crystallization.

(bl) After the raw material is supplied, the liquid supply valve V is closed, the piston (4) is lowered to pressurize the raw material in the container (9), and the crystallization of the specific component is promoted. ) is in a solid-liquid coexistence state (
solid-liquid mixture).

(C1 After the above crystallization, the drain valve ■2 is opened and the liquid phase is discharged under pressure to the outside of the container (9), forming a solid phase of the specific component in the container (9). Normal case Then, the remaining liquid is drained by squeezing the phase contained in the container (9).The liquid phase passes through the filter (2) and is drained from the drain pipe (6) of the lower lid (3) through the gap on the back side of the filter (2). It exits the container (9) through .

(d) After discharging the liquid, as shown in Figure 3, the cylinder (1
), separates from the lower lid (3) to open the inside of the container (9), then advances the chute (8) and advances the bushing (7) to remove the solid phase C (hereinafter referred to as product). ).

tel After taking out the above product, use the chute (8) and
Exit the socha (7), lower the cylindrical body (1), and open the lower lid (
3) to seal the container (9).

After the container (9) is sealed, the process returns to the fat raw material supply process, and the series of operations from the fal process to the tel process are repeated until a predetermined amount of product is obtained.

(Problem to be Solved by the Invention) The time required to perform the above series of operations once (time required per cycle) is usually about 2 to 5 minutes. However, the amount of product produced per cycle is small, and the amount of product produced per unit time (hereinafter referred to as productivity) is low, so the above operations are usually repeated thousands to hundreds of times. There is a problem in that it takes a long time to obtain a fixed amount of product. Therefore, in order to improve productivity, it is strongly desired to shorten the time required per cycle by even a few seconds.

In the above series of operations, in the step (di) related to product removal, the inside of the container (9) is opened, and in the step tel, the container (9) is sealed, so that the pressure crystallization process becomes a Basochi method. Products cannot be produced continuously, and in particular, the process fd)fe) related to product extraction and the raw material supply process (al) take a long time.Therefore, it is necessary to shorten the time required in these processes. ,
It is effective in shortening the time required per cycle and improving productivity.

The present invention was made in view of these circumstances, and its purpose is to solve the above-mentioned problems of the conventional methods and to shorten the time required for the product removal process and the raw material supply process. The present invention aims to provide a pressure crystallizer that can significantly improve productivity.

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

That is, the apparatus according to claim 1 includes a high-pressure container, and a piston that fits into the inner circumference of the container and moves up and down to divide the inside of the container into an upper raw material slurry chamber and a lower separation compression chamber. , a high-pressure pump that supplies and pressurizes the raw material to the raw material slurry chamber;
a solid phase extraction port provided at the lower part of the separation and compression chamber;
A valve rod for opening and closing the solid phase extraction port, a drain pipe connected to the separation and compression chamber via a filter and a liquid phase outlet hole, and a drain valve connected to the drain pipe. A pressure crystallizer having a pressure crystallizer, wherein the piston has a flow path communicating from the raw material slurry chamber to the separation compression chamber, and a valve that opens and closes the flow path. It is an analysis device.

The apparatus according to claim 2 is the pressure crystallizer according to claim 1, wherein a drain pipe is connected to the raw material slurry chamber through a filter and a liquid phase outlet hole.

(Function) Since the pressure crystallizer according to the present invention is configured as described above, it becomes possible to carry out a highly productive pressure crystallization process as described below.

That is, first, the piston is positioned on the road of the high-pressure container, and with the flow path opening/closing valve in the piston open, the high-pressure pump supplies the raw material to the raw material slurry chamber, and the slurry chamber and the separated compression After supplying the raw material to the chamber, the flow path opening/closing valve is closed.

Next, the drain valve of the drain pipe connected to the separation and compression chamber via the filter and the liquid phase discharge hole is opened, and the raw material is supplied to the raw material slurry chamber by the high-pressure pump, so that the raw material supply pressure As a result, the piston is pushed down, and the liquid phase can be discharged out of the separation and compression chamber through the filter and the liquid phase discharge hole, and as a result, the solid phase of the specific component remains. Alternatively, it is also possible to further compress the solid phase and discharge the liquid phase.

After the formation of the solid phase component, the drain valve of the drain pipe is closed, and the valve rod that opens and closes the solid phase extraction port at the bottom of the separation and compression chamber is operated to open the extraction port, and the piston is moved. When it is lowered, the solid phase (ie, product) is crushed and taken out from the extraction port to the outside of the separation and compression chamber.

In parallel with the liquid phase discharging step in the separation and compression chamber, or further in parallel with the product take-out step, the raw material can be supplied to the raw material slurry chamber by a high-pressure pump. Therefore, after the product is taken out, the raw material slurry chamber, which has increased in volume, is filled with raw material.

After taking out the product, when the piston is raised with the solid phase extraction port closed and the flow path opening/closing valve in the piston opened, the raw material in the raw material slurry chamber can be injected into the separation and compression chamber.

After that, the flow path opening/closing valve is closed, the drain valve of the drain pipe is opened, and while the raw material is supplied to the raw material slurry chamber by the high-pressure pump, the liquid phase is discharged to the outside of the separation and compression chamber. Repeat the series of operations from step to product removal step.

As described above, since it is not necessary to open the inside of the high-pressure container to take out the product, the time required for the product removal process is shortened. In addition, in parallel with the liquid phase discharging process and product extraction process in the separation and compression chamber, raw materials can be supplied to the raw material slurry chamber by a high-pressure pump, and raw material injection into the separation and compression chamber can be started immediately after product extraction. . Furthermore, since this raw material injection occurs as the piston rises, the time required for raw material injection is included in the time required for the piston to rise, and is substantially reduced to almost nothing. Therefore, the time required per cycle can be significantly shortened, and as a result, productivity can be greatly improved.

Further, according to the pressure crystallizer according to the present invention, the following pressure crystallization process can also be carried out.

That is, first, the piston is positioned approximately at the lower part of the high-pressure container, and after supplying the raw material to the raw material slurry chamber by the high-pressure pump, the piston is positioned at approximately the center of the high-pressure container with the flow passage opening/closing valve inside the piston being opened. When the slurry chamber is raised to approximately half of the raw material in the slurry chamber, approximately half of the raw material in the slurry chamber can be injected into the separation and compression chamber. Next,
When the piston is lowered with the flow path opening/closing valve closed, the raw material in the separation and compression chamber is pressurized, causing crystallization of a specific component.

After the crystallization, when the drain valve of the drain pipe is opened, the liquid phase can be discharged and a solid phase of the specific component can be formed in the separation and compression chamber. Alternatively, it may be further compressed. Thereafter, by opening the solid phase extraction port at the bottom of the separation and compression chamber and lowering the piston, the solid phase (product) can be taken out without being crushed.

In parallel with the pressurized crystallization process, liquid phase discharge, and product take-out process in the separation and compression chamber, raw materials can be supplied to the raw material slurry chamber by a high-pressure pump to fill the chamber.

After taking out the product, since the raw material has already been filled in the raw material slurry chamber, the raw material can be immediately started to be injected into the separation and compression chamber by raising the piston in the same way as described above, and from then on, the process starts from this raw material injection step to the product unloading step. A series of operations (the process of supplying the raw material to the raw material slurry chamber is performed in parallel) is repeated.

With such a process, the time required for the product extraction process is shortened, and the time required for raw material injection is also reduced to almost nothing, so that the time required per cycle can be significantly shortened.

In the pressure crystallizer according to the present invention, it is preferable that a drain pipe is connected to the raw material slurry chamber through a filter and a liquid phase discharge hole. In this way, when the piston rises and the raw material is injected into the separation and compression chamber, the liquid can be discharged from the raw material slurry chamber, thereby increasing the raw material slurry concentration.
Moreover, pressurization of the raw material can be started while the amount of raw material slurry injected into the separation and compression chamber is always kept constant, and as a result, productivity can be further stabilized.

Providing means for heating the solid phase extraction port near the solid phase extraction port heats the solid phase layer near the solid phase extraction port and reduces the strength of the solid phase layer. ) The upper limit value of the take-out speed can be increased, and therefore productivity can be further improved.

If a valve rod that opens and closes the solid phase extraction port is used that can change its opening degree using an electric signal, it becomes possible to automatically control the product extraction speed.

The arrangement of the high-pressure containers is not limited, and they can be arranged with their axes vertical, horizontal, or inclined.

The inner shape of the high-pressure container is most preferably circular from the viewpoint of pressure resistance, but is not particularly limited.

(Examples) Example 1 A sectional view of essential parts of a pressure crystallizer according to Example 1 is shown in FIG. In FIG. 1, GO+ is a circular vertical high-pressure container, and a piston (IZ) that fits into the inner circumference of the container α0) and moves up and down is provided, dividing the inside of the container GO into two upper and lower chambers. , a raw material slurry chamber is formed in the upper part, and a separation compression chamber α3 is formed in the lower part.

The piston a2 has a flow path (19) that communicates from the raw material slurry chamber (141 to the separation and compression chamber a3), and a valve V that opens and closes the flow path Q91. The container (10) can be driven from outside by a drive rod (1) 1.

Valve V3 can be operated from outside the container αα by means of a connecting rod R connected thereto.

An extrusion die D is provided at the bottom of the separation compression chamber C[3, forming a solid phase extraction port ω, and a valve rod (Is) for opening and closing the extraction port ω is provided at the bottom of the extrusion die D. container (
10) A cylindrical filter (2) is provided on the inner circumference, and a liquid phase discharge hole (21) is provided in the extrusion die D.
Connect the drain pipe (6) to the skeleton (6), and connect the high-pressure automatic valve to the skeleton (6).
, and connected to tank T1 via nozzle N1, and
A heater H is incorporated inside the die D.

A high pressure pump αG for supplying and pressurizing the raw material to the chamber α4 and a raw material tank (not shown) are connected to the raw material slurry chamber by pipes. A filter a and a liquid phase discharge hole (22) are provided at the top of the slurry chamber (14J), a drain pipe og is connected to the discharge hole (22), and the skeleton a8 is equipped with a high-pressure automatic valve (2) and a nozzle. It is connected to the tank T2 via N2.The drain pipe qε and the drain pipe (6) communicate with each other via a high-pressure automatic valve (6).

Using the above apparatus, a slurry-like raw material mixture that had been cooled in advance to precipitate seed crystals of a specific component was subjected to pressure crystallization for the purpose of continuously producing a product with a specific component.

First, the above raw materials are introduced into the raw material tank, the solid phase extraction port (■) is made idle with the valve stem αS, and the piston α2 is positioned at the bottom of the container αα. The raw material was supplied.Next, the automatic valve 6 was opened to communicate the drain pipe αg and the drain pipe (6), and the piston Q2 was opened with the valve 2 of the piston flow path Q9) open.
was raised to the center of the container α0), and half of the raw material in the slurry chamber α4 was injected into the separation and compression chamber α3 via the flow path α9. In addition, the reason why the automatic valve V was opened is to keep the raw material slurry chamber Q41 and the separation compression chamber α3 at the same pressure, and to open the piston α2.
This is to make it easier to rise.

After the raw material was injected, the valve (1) of the flow path (1g) was closed, and in this state, the piston +12 was lowered to pressurize the raw material in the separation compression chamber C13 to 1500 atm and crystallize it. Next, the valve (2) of the drain pipe (6) was opened to discharge the liquid phase to the tank T, forming a solid phase in the separation and compression chamber α3.

Next, the heater H of the die D is energized to heat the valve stem α9.
was lowered to open the outlet υ, and the piston a was lowered to crush the solid phase (product) and take it out of the separation and compression chamber q3 from the outlet (2).

On the other hand, in parallel with the pressurized crystallization and liquid phase discharge steps in the separation and compression chamber CI3, raw material was supplied into the raw material slurry chamber αΦ by a high-pressure pump (NG) to fill the raw material slurry chamber αΦ.

After the product is taken out, since the slurry chamber a4 is already filled with the raw material, the raw material injection into the separation compression chamber α3 is immediately started by raising the piston a2 in the same manner as described above, and from then on, the product is taken out from this raw material injection process. A series of operations leading up to the process (the raw material supply process to the raw material slurry chamber was performed in parallel) were repeated.

As a result, compared to the case using conventional equipment, the time required per cycle was significantly shortened, and productivity was improved.

Example 2 A slurry-like raw material containing 50% crystals of a specific component was prepared in advance by pressure crystallization using a pressure means outside the high-pressure container, and solid-liquid separation was performed using the pressure crystallizer according to Example 1. A process was implemented.

First, the piston α2 is positioned at the upper part of the container αα, and with the valve V of the flow path α9) of the piston open, raw materials are supplied by a high-pressure pump (IG) to the raw material slurry chamber α4 and the separation compression chamber α3. After filling the tank, close the valve v3. Next, open the valve ■4 of the drain pipe (6) and turn off the high pressure pump q.
The raw material was supplied to the raw material slurry chamber α fathom by e, the piston uz was pushed down, the liquid phase was discharged, and the mixture was further compressed.

Next, close the valve v4 of the drain pipe (6), lower the valve stem a9 to open the outlet ■, lower the piston α, and crush the solid phase (product). It was taken out from the extraction port ■ to the outside of the separation compression chamber α3.

After taking out the product, close the solid phase extraction port (■), open the valve v3 of the piston flow path α9), raise the piston α2, and separate the raw material in the raw material slurry chamber α into the compression chamber α3.
injected into.

After this, the valve ■ of the piston flow path α9 is closed, the valve v4 of the drain pipe is opened, and the raw material slurry chamber α4 is operated by the high pressure pump αG.
The liquid phase was discharged outside the separation and compression chamber qJ while the raw material was being supplied to the chamber, and thereafter a series of operations from this step to the product removal step were repeated.

As a result, the time required per cycle could be reduced compared to the case of Example 1.

(Effects of the Invention) According to the pressure crystallizer according to the present invention, the time required for the product take-out process and the raw material supply process can be shortened, and therefore l
Significantly reduces the time required per cycle, increasing productivity (
The amount of product produced per unit time can be greatly improved.

[Brief explanation of drawings]

FIG. 1 is a sectional view of a main part of a pressure crystallizer according to Example 1, FIG. 2 is a sectional view of a main part showing a typical example of a conventional pressure crystallizer,
FIG. 3 is a cross-sectional view of the main parts showing the situation when taking out the product when using the above conventional device (1) - Pressure-resistant cylinder (3) - Lid (5) - Raw material supply pipe (7) - Pressure container (9) - Pressure resistant container α toe drive rod (+3 - Separate compression chamber α5 - Valve rod αη - Filter α9 - Channel (21) - Liquid phase discharge hole ■1 - Liquid supply valve v, - Valve C - Product H - Heater N1.N2 - Nozzle (2) - Cylindrical filter (4) - Piston (6) - Drain pipe (8) - Chute α0) - High pressure container α2 - Piston a fathom - Raw material slurry chamber αG - High pressure pump decoy - Drain pipe ■ - Solid phase extraction port (22) - 1 liquid phase discharge hole Vz - 1 drain valve V4. Vs, L - High pressure automatic valve - Extrusion die R Series connecting rod T, T, - 1 tank Figure 1 Patent applicant: Kobe Steel Oriyoshi Co., Ltd. Patent attorney: Akira Kanamaru

Claims (2)

[Claims] (1) A high-pressure container, a piston that fits into the inner circumference of the container and moves up and down to divide the inside of the container into an upper raw material slurry chamber and a lower separation compression chamber, and a piston that moves raw materials into the raw material slurry chamber. A high-pressure pump that supplies and pressurizes the air, a solid phase extraction port provided at the bottom of the separation and compression chamber, a valve rod that opens and closes the solid phase extraction port, and a filter and liquid phase discharge to the separation and compression chamber. A pressure crystallizer having a drain pipe connected through a hole and a drain valve connected to the drain pipe, wherein the piston communicates from the raw material slurry chamber to the separation compression chamber. 1. A pressure crystallizer comprising: a flow path that opens and closes the flow path; and a valve that opens and closes the flow path. (2) The pressure crystallizer according to claim 1, wherein a drain pipe is connected to the raw material slurry chamber via a filter and a liquid phase discharge hole.