JPH0286802A - Pressure crystallizer - Google Patents

Abstract

PURPOSE:To reduce the repeated operating time by providing a cylindrical sealing member which is engaged with the inner peripheral wall of a pressure cylinder on the piston inlet side and the outer periphery of the piston, reciprocated independently of a piston member, and used for closing or opening a raw material supply port. CONSTITUTION:The pressure cylinder 1 a cap 3 opposed to the opening of the cylinder 1 on one side, and the piston 4 opposed to the opening of the cylinder 1 on the other side and reciprocating in the cylinder 1 are provided. The cylinder 1 or the cap 3 is made free to reciprocate in the axial direction of the cylinder 1. The cylinder 1 cap 3, and piston 4 are arranged so that the respective axes are horizontally directed, and the raw material supply port 19 is formed in the inner peripheral wall of the cylinder 1 on the piston 4 inlet side. The cylindrical sealing member 9, which is engaged with the inner peripheral wall and the outer periphery of the piston 4, reciprocated independently of the piston 4 member, and used for closing or opening the supply port 19, is provided. As a result, the time necessary for the repeated operating cycle can be reduced, and the purity of the product can be improved.

Description

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

(Conventional technology) Pressure crystallization has great potential for application to raw material systems that are difficult to separate using conventional distillation or cooling crystallization, is easy to obtain high-purity products, and has high Due to its easy yield and low energy consumption, 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.

A typical example of a conventional apparatus used in such a pressure crystallization method is shown in FIG. 5. In FIG. It is arranged so that (2) is a cylindrical filter for solid-liquid separation arranged on the inner peripheral wall of the pressure-resistant cylinder (1), and (3) is a lid body ( lower lid)
, (4) is a pressurizing/squeezing piston inserted from the upper opening of the pressure-resistant cylinder (1), (5) is a raw material supply pipe, V,
is a liquid supply valve provided in the raw material supply pipe (5), (6) is a liquid drainage passage, v2 is a liquid drainage valve provided in the liquid drainage passage (6), (
7) shows a bushing for taking out the crystallized substance, and (8) shows a chute for taking out the crystallized substance.

As described above, the conventional device is one in which the pressure-resistant cylindrical body and the piston axis are arranged in the vertical direction (vertical type).

A representative example of the procedure 111I for performing pressure crystallization using the apparatus shown in FIG. 5 will be described below.

(a) With the drain valve v2 closed, the liquid supply valve v1 is opened to supply the raw material from the raw material supply pipe (5) into the pressure-resistant cylinder (1).

(b) When the supply is finished, close the liquid supply valve v1, and in this state move the piston (4) down next to it to apply high pressure to the raw material in the pressure-resistant cylinder (1) to promote crystallization of specific components. let

(c) When the crystallization is finished, the drain valve ν is opened to proceed to the filtration/squeezing process. In this step, a squeezing force is applied within the pressure-resistant cylinder (1) to discharge the liquid through the filter (2). This liquid is discharged from a gap provided on the back side of the filter (2) through a drain passageway (6) of the lower lid (3).

(d) 'a After passing and squeezing, as shown in Figure 6, the pressure-resistant cylinder (1) is raised to open the inside of the cylinder (1), and then the chute (8) is advanced and the button is pressed. (7)
advance to take out the crystallized product (cake) C.

After completing step (d) above, return to step (a) again and repeat this operation to separate and separate the specific component.
Collection occurs continuously.

(Problem to be Solved by the Invention) However, in the conventional pressure crystallizer as described above, the pressure-resistant cylinder is Since the high pressure loaded in (1) also acts on the raw material supply pipe (5), the passage cross-sectional area of the raw material supply pipe (5) cannot be made sufficiently large, and as a result, the raw material supply takes a considerable length of time. The problem is that it takes time.

Further, when taking out the cake C in the step (d), the chute (8) is advanced and the bushing (7) is advanced. After taking out the cake C, the pressure-resistant cylinder (1)
The chute (
There is a problem in that it is necessary to remove the chute (8) and the button (7), and it takes a considerable amount of time to move the chute (8) and button (7) back and forth.

The above problems lead to the problem that the time required for the repeated operation cycle is long.

In addition, since the conventional pressure crystallizer is a vertical type, the inside of the pressure-resistant cylinder (1) is The residual liquid falls and falls on cake C, so cake C
That is, there is a problem that the purity of the product decreases.

Furthermore, since the device is vertical, from the viewpoint of operability, the forward and backward strokes of the pressure-resistant cylinder (1) and the piston (4) cannot be made sufficiently long, and as a result, the piston (4) cannot be retracted to the highest position. Even if the pressure-resistant cylinder (1) and the piston (4) are fitted together, it is easy to clean or replace the filter (2), etc. inside the pressure-resistant cylinder (1). The problem is that it cannot be done.

The present invention was developed in view of these circumstances, and its purpose is to solve the above-mentioned problems of conventional products, shorten the time required for repeated operation cycles, and improve product purity. It is an object of the present invention to provide a pressure crystallizer in which the interior of the pressure-resistant cylinder can be easily maintained and managed.

(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 pressure-resistant cylinder, a lid facing an opening on one side of the pressure-resistant cylinder, and an opening on the other side of the pressure-resistant cylinder, and A pressure crystallizer comprising a piston that moves forward and backward within a pressure-resistant cylinder, and in which at least one of the pressure-resistant cylinder or the lid is movable in the axial direction of the pressure-resistant cylinder,
The pressure-resistant cylindrical body, the lid body, and the piston are arranged so that their respective axes are in the horizontal direction, and a raw material supply port is formed on the inner circumferential wall of the pressure-resistant cylindrical body on the piston entry side. The pressure crystallizer is characterized in that it includes cylindrical seal members that fit into the outer circumferential portions of the pistons and move back and forth independently of the piston members to close or open the supply ports.

(Function) As explained above, in the pressure crystallizer according to the present invention, a raw material supply port is formed on the inner circumferential wall of the pressure-resistant cylinder on the piston entry side, and furthermore, the raw material supply port is formed on the inner circumferential wall and the outer circumferential portion of the piston. A cylindrical seal member is provided which is fitted into the supply port and moves back and forth independently of the piston member to close or open the supply port. Therefore, the opening on the inner wall side of the raw material supply port (hereinafter referred to as supply port) can be closed by this cylindrical seal member. In this closed state, high pressure is applied to the pressure-resistant cylinder for crystallization, filtration, and squeezing.
Since this high pressure does not act on the supply port, the cross-sectional area of the supply port can be made sufficiently large. This makes it possible to shorten the raw material supply time.

Furthermore, when the raw material is supplied in the form of a slurry, it becomes possible to eliminate the clogging accident of the raw material supply pipe that is often experienced in conventional devices.

Further, a pressure-resistant cylinder, a lid, and a piston are arranged so that their axes are in the horizontal direction (horizontal type) 6. In addition, the pressure-resistant cylinder or the lid (one of which can move forward and backward in the axial direction of the pressure-resistant cylinder, and the piston can move forward and backward within the pressure-resistant cylinder.
After the compression is completed, the pressure-resistant cylinder can be horizontally retracted from the lid, or the lid, cake C, and piston can be horizontally retracted from the pressure-resistant cylinder. In this way, the cake C is held between the lid and the piston, and there is no pressure-resistant cylinder around the cake C. Next, when the piston is retracted, the cake C will fall under its own weight (that is, the cake C will be taken out). In this way, cake C can be taken out by moving at least two sides of the pressure-resistant cylinder or the lid and moving the piston back and forth, and can be done without using the chute (8) and pusher (7). . Therefore, the cake C can be taken out easily and in a short time.

In addition, since the pressure crystallizer according to the present invention is of a horizontal type as described above, the residual liquid in the pressure-resistant cylinder does not fall during the step of taking out the cake C, so there is a problem of a decrease in the purity of the cake C due to the residual liquid. The points are cleared.

Furthermore, since the pressure crystallizer according to the present invention is horizontal as described above, there is no height restriction, and the forward and backward strokes of the pressure-resistant cylinder and the piston can be made sufficiently long. As a result, the pressure-resistant cylindrical body and the piston can be separated from each other, making it easy to clean and replace filters and the like inside the pressure-resistant cylindrical body. Furthermore, since it is horizontal, the length (height) of the device can be reduced, which further facilitates cleaning of the inside of the pressure-resistant cylinder.

In addition, since at least one of the pressure-resistant cylinder and the lid body is movable in the axial direction of the pressure-resistant cylinder, both may be made movable, or only one of them may be movable. Good too. Which of these configurations should you choose?
The selection should be made depending on the situation at the installation site.

Regarding the method of injecting the raw material (slurry liquid), since the cross-sectional area of the supply port can be made sufficiently large, the raw material may be injected using its own weight, or it may be injected using a pressurizing means.

Regarding the inner shape of the pressure-resistant cylindrical body, from the viewpoint of pressure resistance, it is most desirable to have a circular shape, but in some cases, it may be an ellipse, or it can also be a polygonal shape such as a hexagon.

The sealing member closes the opening on the inner wall side of the supply port when the sealing member is fitted to the inner circumferential wall of the pressure-resistant cylinder. In order to achieve this function, a sealing puncture may be provided between the inner wall side opening of the supply port and the pressure-resistant cylinder body to which high pressure is applied. There are no particular restrictions on the shape or structure of this packing, and any known packing can be used.

Moreover, as a means for moving the piston, pressure-resistant cylinder, etc. forward and backward, a hydraulic cylinder or other movement means such as a solenoid mechanism can be employed.

(Example) Embodiments according to the present invention will be described with reference to the drawings.

Actual Figures 1 to 4 show partially cutaway side views of the pressure crystallizer according to the first embodiment. In these figures, (1) is a pressure-resistant cylindrical body, which is arranged so that its axis is in the horizontal direction. (2) is a cylindrical filter for solid-liquid separation installed on the inner peripheral wall of the pressure-resistant cylinder (1); (3) is the pressure-resistant cylinder (1);
) is a good example (left side in the figure) of the lid body facing the frontage, and (4) facing the opening of the other side (right side in the figure) of the pressure-resistant cylinder (1), and the inside of the pressure-resistant cylinder A piston for pressurizing and squeezing that moves back and forth, (5) is a raw material supply pipe, (6) is an IJl-liquid passage, (9) is a cylindrical seal member, (LQa)
and (10b) is a press frame, (11) is a slide par,
The surface and Q31 are 1941 members, θ4. θ9 and 0θ are hydraulic cylinders, θ is a hopper, 08) is a raw material reservoir, and S is a sealing punch.

In this way, the pressure crystallizer according to Example 1 has a press frame (
LOa) and (10b) are integrally attached via four slide pars 61). A lid (3) is fixed to this press frame (10a) with its axis horizontal. The press frame (10b) is provided with a hydraulic cylinder, and a piston (4) for pressurizing and squeezing is provided so as to face the lid (3) and move back and forth concentrically therewith. ing.

In addition, the slide member 01) is arranged so as to be slidable on both sides, and a pressure-resistant cylinder (1) is arranged concentrically with the piston (4) in the center of the slide member 02). At the same time, a raw material reservoir 00 is attached, and the hydraulic cylinder 04) is configured to be movable in the left-right direction (axial direction) in the drawing.

On the other hand, a cylindrical seal member (9) is fixed concentrically to the pressure-resistant cylinder (1), lid (3) and piston (4) at the center of the slide member OQ, and is axially fixed by a hydraulic cylinder 0ω. It is configured to be able to move toward the heart.

Further, a cylindrical filter (2) is attached to the inner circumferential wall of the pressure-resistant cylinder (1) on the lid (3) side. The opposite side, that is, the inner circumferential wall on the entry side of the piston (4) is formed to have an inner diameter larger than the diameter of the piston (4), and the large inner diameter portion is provided with a raw material supply port side.

On the other hand, the cylindrical sealing member (9) disposed on the right side of the pressure-resistant cylinder (1) in the drawing tightly fits into the large inner diameter part of the pressure-resistant cylinder (1), and the outer peripheral part of the piston (4). It is configured to fit into the piston (4) and move back and forth independently of the piston (4) to close or open the opening on the inner wall side of the supply port 09.

As explained above, the pressure crystallizer according to Example 1 is
The pressure-resistant cylinder (1), the piston (4), etc. are arranged so that their axes are in the horizontal direction (horizontal type).

Using this pressure crystallizer, pressure crystallization was performed in the following manner. That is, as shown in FIG.
, move the slide member 02) to the left in the drawing,
The left end opening of the pressure-resistant cylinder (1) is fitted into the lid (3). At this time, the piston (4) has retreated to the right side,
Further, the cylindrical seal member (9) is also retracted to the right, and the supply port 09 is opened in the pressure-resistant cylinder (1). In this state, the raw material is injected into the pressure-resistant cylinder (1).

After the raw material is injected, the hydraulic cylinder 06) is operated to advance the cylindrical seal member (9) along with the slide member to the left in the drawing, and its outer peripheral surface is fitted into the large inner diameter portion of the pressure-resistant cylinder (1). By doing so, the supply port 09) is closed and the inside of the pressure-resistant cylinder (1) is sealed.

After that, actuate the hydraulic cylinder 04 to move the piston (4).
was applied, and pressure crystallization, filtration, and compression were performed according to conventional methods. This situation is shown in Figure 3.

After the compression was completed, the pressure-resistant cylinder (1) and the cylindrical seal member (9) were retracted to the right in the drawing while the piston (4) remained advanced. In this way, the cake C is sandwiched between the lid and the piston.

Next, as shown in FIG. 4, the piston was retracted and cake C was dropped onto the hopper.

Next, this cake C is carried out, and the piston (4
) was retracted to the right in the drawing, and the pressure-resistant cylinder (1) was advanced to the left in the drawing, and its left end was fitted into the lid (3). This operation brings the pressure crystallizer into the state before the raw material injection described in FIG. 2 above. Thereafter, raw materials were injected into the pressure-resistant cylinder (1), pressure crystallized, IF filtered and squeezed, and cake C was dropped and carried out in the same manner as described above.

This series of operations was then repeated. As a result, compared to pressure crystallization using conventional equipment, the time required for repeated operation cycles was significantly shortened by several percent to several tens of percent. Additionally, product purity was improved. Furthermore, the interior of the pressure-resistant cylinder was inspected during the repetition of the above operations, and the inspection was extremely easy.

(Effects of the Invention) According to the pressure crystallizer according to the present invention, the raw material supply time can be shortened, and the cake C can be taken out quickly and easily, so the time required for repeated operation cycles is reduced. can be significantly shortened and productivity can be extremely high. Furthermore, since the problem of reduced product purity due to residual liquid in the pressure-resistant cylinder is resolved, product purity can be improved. Furthermore, maintenance, inspection, etc. inside the pressure-resistant cylinder can be easily performed.

In addition to the above, when the raw material is supplied in the form of a slurry, there is also the effect that it is possible to eliminate the clogging accident of the raw material supply pipe that is often experienced in conventional devices.

[Brief explanation of the drawing]

Figures 1 to 4 are partially cutaway side views of the pressure crystallizer according to Example 1, and Figure 5 is a representative of a conventional apparatus used in the pressure crystallization method. A diagram showing an example, FIG. 6, is a diagram showing a situation when taking out a crystallized product obtained by the conventional apparatus. (IL- (IQb) θ21031 Qη Pressure-resistant cylindrical body lid body - raw material supply pipe pusher cylindrical seal member - press frame slide member hopper raw material supply port drain valve seal seal (21 --- one cylindrical filter (41 ----Piston (61---Drain passage (8)---Shade (10a)---Press frame G11---Slide bar 041 G51061-1 Mountain pressure cylinder (l[1l--
- One raw material reservoir V, - One liquid supply valve C - One cake Patent applicant Kobe Steel Co., Ltd. Agent Patent attorney Akira Kaneki -

Claims (1)

[Claims] (1) a pressure-resistant cylinder, a lid facing the opening on one side of the pressure-resistant cylinder, and a lid facing the opening on the other side of the pressure-resistant cylinder;
In the pressure crystallizer, the pressure crystallizer includes a piston that moves forward and backward within the pressure-resistant cylinder, and at least one of the pressure-resistant cylinder or the lid is movable in the axial direction of the pressure-resistant cylinder. , a lid body and a piston are arranged so that their axes are horizontal, a raw material supply port is formed on an inner circumferential wall on the piston entry side of the pressure-resistant cylinder, and the inner circumferential wall and an outer circumferential portion of the piston are connected to each other. 1. A pressure crystallizer comprising a cylindrical seal member that is fitted into each of the piston members and moves back and forth independently of the piston member to close or open the supply port.