JPH02169003A - Apparatus and process for pressure crystallization - Google Patents

Abstract

PURPOSE:To shorten the time for separating the solid phase in a pressure crystallization apparatus provided with a filter for discharging the liquid phase on the inside of the cylinder and/or the surfaces pressed by pistons, by forming a hole for discharging the solid phase in the manner to penetrate the wall or the pressure-resistant cylinder body. CONSTITUTION:A first piston 10 moving to and fro in the inside of a cylinder body 11 from an opening at one side of a pressure resistant cylinder body 11, and a second piston 15 moving to and fro in the inside of the cylinder body 11 from an opening at another side of the cylinder body 11 are provided. Further, a filter 12, 16 for discharging a liquid phase is provided to the inside of the cylinder body 11 and/or a surface pressed by the piston. Further, a hole 13 for discharging a solid phase penetrating a cylinder wall is provided to the pressure resistor cylinder body 11. As the result, a time required for discharging the solid phase is shortened, and the time required for repeating the operation cycle is shortened. Moreover, the purity of the product is improved. Furthermore, the discharge of the solid phase is facilitated even if a level of the solid phase after the solid/liquid separation is low, or the solid phase is soft or semi- solid.

Description

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

(Prior art) Pressure crystallization has great potential for application to raw material systems 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, as it is easy to obtain high yields and consumes little energy.

A typical example of a conventional apparatus used in such a pressure crystallization method is shown in FIG. In Figure 1.1, (+) is a pressure-resistant cylindrical body constituting a pressure-resistant container, (2) is a cylindrical filter for solid-liquid separation arranged on the inner peripheral wall of the cylindrical body (1), and (3) (4) is a pressure-resistant cylinder (11) with a lid that is tightly fitted into the lower opening, (4) is a pressurizing/squeezing piston that is fitted into the upper opening of the pressure-resistant cylinder (1), (5) is a Raw material supply pipe, V is liquid supply valve,
(6) is a drain passage, V is a drain valve, (7) is a button for taking out crystallized substances, and (8) is a chute for taking out crystallized substances.

A typical example of the procedure for performing pressure crystallization using the apparatus shown in FIG. 11 will be described below.

(a3 With the drain valve V! closed, open the liquid supply valve v1 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 V, and in this state lower the piston (4) to apply high pressure to the raw material in the pressure-resistant cylinder (1) to promote crystallization of specific components. let

(C) When crystallization is finished, drain valve v2 is opened to discharge the liquid phase out of the container under pressure to separate solid and liquid. In normal cases, after the separation, the solid phase in the container is further compressed to discharge the remaining liquid (hereinafter, even when compression is performed in this way, it is also referred to as solid-liquid separation).In addition, when compression is not performed There is also.

In this solid-liquid separation step, pressure 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) After separation at night, as shown in Figure 12, 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 removed. (7) is advanced to take out the crystallized product (solid phase component) 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 crystallization apparatus and method as described below, when performing the solid phase separation in the step (d), the cylindrical body ( 1) Since it is necessary to open the inside and advance the chute (8) and bushing, there is a problem that it takes a considerable amount of time to extract the solid phase. In addition, after removing the solid phase, the chute (8) and bushing (7) are removed,
Since the cylindrical body (1) must be lowered and fitted with the lower cover (3), this also requires a considerable amount of time. The above-mentioned problems lead to the problem that the time required for the repeated operation cycle becomes long and productivity deteriorates.

In addition, during solid phase extraction, residual 'lFi (containing impurities) in the cylinder (1) drips between the time when the cylinder (1) starts to rise and the time when the solid phase extraction is completed. , there is a problem that the purity of the solid phase component (product) decreases because it concentrates on the solid phase component.

Furthermore, if the solid phase concentration (concentration) in the solid-liquid coexistence mixture after crystallization is low (for example, 25% or less), the height of the solid phase component after the solid-liquid component # will be low. However, there is a problem in that the solid phase cannot be easily extracted. In addition, if the crystal grain size of the solid phase component is small (observed in the case of pressure crystallization of aliphatic compounds, etc.) or if the purity of the solid phase component (product) is low, the solid phase component after solid-liquid separation may The problem is that the phase becomes soft or semi-solid like shearbent, and in such a case, it is extremely difficult to extract the solid phase without introducing impurities.

The present invention has been made in view of these circumstances, and its purpose is to solve the above-mentioned problems of conventional methods, shorten the solid phase extraction time, and eliminate the need for repeated commercial cycles. It can shorten the time, improve product purity, and reduce the height of the solid phase after solid-liquid separation.
It is an object of the present invention to provide a pressure crystallization apparatus and method that can easily extract a solid phase even when the solid phase is soft or semi-solid.

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

That is, the device according to the present invention includes a pressure-resistant cylinder, a first piston that moves forward and backward within the cylinder through an opening on one side of the cylinder, and a first piston that moves forward and backward within the cylinder through an opening on the other side of the cylinder. A pressure crystallizer comprising a second piston, and a filter for discharging a liquid phase component is disposed inside the cylinder and/or on the piston pressing surface, the pressure crystallizer having a second piston and a filter for discharging a liquid phase disposed on the inside of the cylinder and/or the piston pressing surface, the pressure crystallizer having a second piston that penetrates the cylinder wall into the pressure-resistant cylinder. This is a pressure crystallizer characterized by being provided with a hole for extracting a solid phase component.

The method according to the present invention involves inserting a first piston and/or a second piston into a pressure-resistant cylinder to form a container, supplying the raw material 14 to the container, and pressurizing it to form a mixture in a solid-liquid coexistence state. This is a pressure crystallization method in which the liquid phase is subsequently discharged to the outside of the container under pressure to separate solid and liquid, and then the solid phase is taken out of the container, the solid phase being transferred to a first piston and a second piston. This is a pressure crystallization method characterized in that the solid phase is taken out by moving it to a hole for taking out the solid phase of a pressure-resistant cylinder and extruding it from the hole.

(Function) As explained above, the pressure crystallizer surface according to the present invention includes a pressure-resistant cylinder (hereinafter referred to as cylinder) equipped with a hole for solid phase extraction, and a first cylinder that moves forward and backward inside the cylinder. Piston and second screw]・
In addition, a liquid phase discharge filter is disposed inside the cylinder and/or on the piston pressing surface.

Therefore, when the first piston and/or the second piston are inserted into the cylinder to form a container and the raw material is supplied to the container, the raw material can be pressurized. Therefore, it forms a mixture in which solid and liquid coexist and can be separated into solid and liquid.

The above-mentioned container formation and raw material supply can be performed as follows. Therefore, if the device is vertical (the axis of the pressure-resistant cylinder is vertical) and the solid phase extraction hole (hereinafter referred to as the extraction hole) is located at the top of the cylinder, there is a hole at the bottom of the cylinder. Insert the piston, and if the extraction hole is located at the bottom of the cylinder, insert the lower piston to the position where the hole is closed, and then inject the raw material.

If the device is horizontal and the extraction hole is on the right side of the cylinder, insert both the left and right pistons until they do not close the extraction hole.
After injecting the raw material from the extraction hole, insert the right piston to the position where the extraction hole is closed.If the piston has a raw material supply pipe passing through it, insert both pistons (the right piston should be in the extraction hole closed position). (inserted until the end), then inject 1 liter of raw material from the raw material supply pipe.

After the solid-liquid separation, the solid phase is moved to the extraction hole of the cylinder by the first piston and the second screw, and when a force is applied to the solid phase, the solid tI is pushed out from the step hole, It can be taken out. At this time, if the solid phase is soft, it is like a fluid, and conversely, if the solid phase is a hard solid, the solid is crushed and extruded.

The solid phase component can be taken out and moved to the flower part, for example, while the solid phase component is being held between the first piston and the second piston, and can be carried out instantaneously and easily. Further, the time required for extrusion can be shortened by increasing the piston pressing force and/or by increasing the cross-sectional area of the side hole. Therefore, the solid phase extraction time can be shortened.

After taking out the solid phase, by moving the piston, the container formation and raw material supply can be performed. This piston movement can also be performed instantaneously and easily.

Therefore, the time required for repeated operation cycles can be reduced,
Productivity can be improved.

In addition, as described above, the solid phase can be moved and extruded while being held between the pistons, so the solid phase can be taken out without dripping residual liquid into the product, improving product purity. become.

Further, as mentioned above, the solid phase fraction can be extracted by moving the solid phase component to the extraction hole and extruding it, and the height of the same integration has no effect on the operability of these operations. Also, the properties of the solid phase (
Hardness, etc.) has an influence on extrudability, and if the hardness is as hard as 4, it will be difficult to extrude, but in such a case, extrusion can be made easier by increasing the pressing force with the piston. Therefore, even when the height of the solid phase after solid-liquid separation is low, or when the solid phase is soft or semi-solid, it is possible to easily extract the solid phase.

Furthermore, if a solid phase separation pipe directly connected to the product storage is connected to the extraction hole, the solid phase component can be recovered without being contaminated by atmospheric dust or the like. Furthermore, since the atmosphere inside the storage and take-out pipe can be adjusted, even in the case of substances that dislike the atmosphere (solid phase components), the solid phase components can be recovered without coming into contact with the atmosphere.

In the pressure crystallization method according to the present invention, pressure crystallization is performed using the same operations as those described in the above description. That is, a first piston and/or a second piston are inserted into a cylinder to form a container, raw F4 is supplied to the container, and is pressurized to form a mixture in a solid-liquid coexistence state. After the phase is discharged out of the container and separated into solid and liquid, the solid phase is moved to the extraction hole of the cylinder by the first piston and the second piston and pushed out from the step hole to take out the solid phase. I try to do this. Therefore, the same effects as described above can be obtained, and productivity and product purity can be improved.

In addition, the said take-out hole can also be used as a raw material supply port as mentioned above. The cross-sectional edge of the step hole can be made sufficiently large. Therefore, when raw materials are supplied through the step hole, the raw material supply time can be shortened, and when raw materials are supplied in slurry form, it is possible to eliminate the clogging accidents of raw material supply pipes that are often experienced in conventional equipment. .

The inner shape of the cylindrical body is most preferably circular from the viewpoint of pressure resistance, but is not particularly limited.

The cylindrical body may be fixed and both pistons may be movable, one piston may be fixed and the cylindrical body and the other piston may be movable, or the cylindrical body and both pistons may be movable.

The means for moving pistons, cylinders, etc. forward and backward are hydraulic cylinders,
Other advancing/retracting means such as a solenoid mechanism may be employed.

(Example) L[Ll A sectional view of the main parts of a pressure crystallizer according to Example 1 is shown in FIG. This device is vertical. In Figure 1, (11)
is a cylindrical body, and a cylindrical filter surface is disposed on its inner surface. At the bottom of the cylindrical body (11), a take-out hole surface is provided at a position one side away from the cylindrical filter installation part, and the take-out hole 03)
The product outlet pipe side is connected to.

An upper piston 00) and a lower piston 0ω are arranged at the upper and lower parts of the cylinder (11). (9L OGI is the cylinder with upper and lower pistons.

A filter 091 is disposed on the pressing surface of the lower piston 09, and a drain passage t2 is provided which passes from the pressing surface to the outside.
I is placed. Q7] is a raw material supply pipe, a field is a heating heater, and a cylinder (11) and a product take-out pipe 0,0
It is placed in the section.

Pressure crystallization was performed using the above apparatus. The main steps of this pressure crystallization are shown in Figures 2-6. First, the lower piston 05 is inserted into the cylinder (11) by a hydraulic cylinder (not shown).
) was advanced until its upper surface was at a position higher than the lower end of the cylindrical filter 07), the extraction hole aω was closed, and a container was formed.

Next, the upper piston 00) is withdrawn from the cylindrical body (11) to open the upper part of the cylindrical body (11), and then the raw material is supplied to the formed container from the raw material supply pipe θ force as shown in FIG. supplied within.

After supplying the raw materials, as shown in Figs. 3 and 4, the upper piston θω
is inserted into the cylinder (1j), the internal weight of the container is pressurized to 1400 atm, and after 5 seconds, the valve of the drain passage 12G is opened to maintain the internal pressure of the container at 1400 atm, and the liquid phase is drained. Discharged outside the container. Subsequently, the solid phase in the container was squeezed to discharge the residual liquid, and the pressure inside the container was lowered stepwise to perform a vacuum sweating process to further purify the solid phase.

”After the sweating process described in Section 2, the upper piston 0ω and the lower piston 0
The solid phase was transferred to the ejection hole 03) while holding the solid phase between 9 and 9 and maintaining a pressure higher than the melting pressure of the solid phase.Then, as shown in Figs. While the piston remains stationary, the upper piston 00) is lowered to crush and extrude the solid phase from the extraction hole side, and the product is extracted T! J
Solid oxide (product) C was taken out through 649.

After removing the solid phase, the valve of the drain passage Q11 is opened, the upper piston 00) is withdrawn from the cylindrical body (11), and the lower piston a0 is moved to the lower end of the cylindrical filter (1). The extraction hole 0 was closed and a container was formed.Through these 12 steps, the state before pouring into the raw material 4 was reached. This series of operations was repeated by carrying out weighted feeding into the tank, applying pressure, and taking out the solid-liquid fraction ^U and the solid phase fraction.

As a result, the time required for the repeating cycle was significantly reduced (40-50%) compared to the conventional case6, and the product purity was improved.

Note that the steps of cofeeding raw material 1, pressurizing, discharging the liquid phase, and squeezing the dotted portion can be repeated several times, and then perform sweating under reduced pressure and take out the product, which will increase the product yield. will improve. In particular, it was confirmed that this method is effective when the solid phase concentration in the raw material is low, and the product yield is significantly improved.

A sectional view of the main parts of the pressure crystallizer according to the second embodiment is shown in FIG. 7. As shown in FIG. 7, the upper piston (IQ) has a raw material supply pipe (21) having a check valve (22). ) is placed inside the piston. The rest is the same as the pressure crystallizer according to Example 1.

With the upper piston 0■ inserted into the cylinder (11),
Advance the lower piston 09, close the extraction hole 03),
After forming the container, the raw material was supplied from the raw material supply pipe (21). After supplying the raw material t:1, pressurization, solid-liquid separation, and solid phase removal were performed in the same manner as in Example 1.

After removing the solid phase, move the upper piston 0ω and the lower piston 0ω to form a container, carry out the steps from supplying raw materials to removing the solid phase in the same manner as above, and repeat this series of operations. Ta.

As a result, compared to the case of the example construction, it is not necessary to withdraw and insert the upper piston 00 into the cylinder (11) when supplying raw t4, so the time required for the repeated operation cycle is further shortened accordingly. .

The raw material supply pipe (21) has a check valve (22) at a position within the piston 0ω, but as shown in Fig. 8, it has an on-off valve (23) instead of the valve (22). A similar effect can be obtained with objects.

Furthermore, as shown in FIG. 9, in the case where a gas supply pipe (24) is provided which branches off from the middle of the raw material supply pipe (21), the upper piston 00) is placed very slightly above the upper limit for liquid phase extraction. If high-pressure gas is purged into the container at the same time, the residual liquid can be discharged more reliably, thereby further improving product purity.

Figure 10 shows a sectional view of the main parts of the pressure crystallizer according to Force LL3 - Example 3. It is a horizontal type device. However, unlike the one shown in FIG. 8, the product outlet tube side is straight.

When raw materials were supplied, pressurized, solid-liquid separation, and solid phase was taken out in the same manner as in Example 2 using the above apparatus, the same results as in Example 2 were obtained.

(Effects of the Invention) According to the pressure crystallizer and method of the present invention, it is possible to shorten the solid phase extraction time, shorten the time required for repeated operation cycles, and prevent residual liquid from dripping onto the product. Product purity can be improved, and even when the height of the solid phase after solid-liquid separation is low, or when the solid phase is soft or semi-solid, it is possible to easily extract the solid phase. Become.

[Brief explanation of the drawing]

Fig. 1 is a sectional view of the main parts of the pressure crystallizer according to the first embodiment, Figs. 2 to 6 are diagrams showing each step of the pressure crystallization according to the first embodiment, and Fig. 7 is a cross-sectional view of the pressure crystallizer according to the second embodiment. Cross-sectional view of the main parts of the pressure crystallizer,
Fig. 8 does not show a pressure crystallizer having an on-off valve (23) instead of the check valve (22) in Fig. 7, and Fig. 9 shows a gas supply branching from the middle of the raw material supply pipe (21). Supply pipe (24)
10 is a diagram showing a horizontal type device in which the device in FIG. The figure shown in FIG. 12 is a diagram showing the situation when taking out the crystallized product obtained by the conventional apparatus. (1) CI+) - Pressure-resistant cylinder (3) - Tom body (5) - Raw material supply pipe line (7) - Bush (9) 00 ~ Cylinder 02) - Cylindrical filter 07 - Product take-out pipe 0ω - 1 Hydraulic cylinder 0 application - Warming heater Ql - Drainage passage (22) - Check valve (24) - Gas supply pipe V, - 1 Drainage valve (2) - Cylindrical filter (4) - Piston ( 6) - Drainage passage (8) - Chute 0ω - Upper piston 0■ - Takeout hole 0ω - Lower piston θ'' 7) - Raw material supply pipe 09 - Filter (21L - Raw material supply pipe (23) - One open/close valve L-1 Liquid Supply Valve C-Cake Patent Applicant Kobe Steel Co., Ltd. Representative Patent Attorney Akira Kanemaru - Figure 7 Figure 8 Figure 2

Claims (2)

[Claims] (1) It has a pressure-resistant cylinder, a first piston that moves forward and backward within the cylinder from an opening on one side of the cylinder, and a second piston that moves forward and backward within the cylinder from an opening on the other side of the cylinder. A pressure crystallizer is provided with a filter for discharging a liquid phase component on the inside of the cylinder and/or on the piston pressing surface, the pressure crystallizer having a filter for discharging a solid phase component that penetrates the wall of the cylinder in the pressure-resistant cylinder. A pressure crystallizer characterized by being provided with holes. (2) A first piston and/or a second piston inside the pressure-resistant cylinder.
A piston is inserted to form a container, the raw material is supplied to the container, pressurized to form a mixture in a solid-liquid coexistence state, and then the liquid phase is discharged outside the container under pressure to separate solid and liquid. , a pressure crystallization method for taking out a solid phase component out of a container, in which the solid phase component is moved to a solid phase extraction hole of a pressure-resistant cylinder by a first piston and a second piston, and is pushed out from the hole. A pressure crystallization method characterized in that the solid phase component is removed by: