JP3662132B2 - Simulated moving bed chromatographic separation system - Google Patents

Description

[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a simulated moving bed type chromatographic separation apparatus, and more particularly to improvement of a rotary valve in the simulated moving bed type chromatographic separation apparatus.
[0002]
[Prior art]
BACKGROUND ART Chromatographic separation apparatuses are widely used in the manufacturing industry such as sugar industry and pharmaceutical industry for the purpose of extracting one or more components from a raw material fluid consisting of a plurality of components obtained by natural or chemical reaction. Various chromatographic separation apparatuses have recently been proposed in addition to the batch fixed bed system conventionally used.
[0003]
FIG. 5 is a schematic sectional view of a separation tower showing the principle of a moving bed type chromatographic separation apparatus. The separation tower 50 is preliminarily filled with a filler (adsorbent) 52 and filled with an eluent. A raw material liquid having two kinds of components A and C is introduced from a raw material supply port F, and an eluent is supplied from an eluent supply port D so as to have a constant linear velocity. The components A and C move at different linear velocities in the separation column 50 due to the difference in affinity with the packing material. For example, the component A having a low affinity moves at a high linear velocity, and the component C having a high affinity has a small line. Move at speed. For this reason, it is separable into the fraction which contains many components A, and the fraction which contains many components C.
[0004]
In the moving bed type separation device, a state is created in which the filler is moved in the direction opposite to the flow of the eluent at a speed intermediate between the moving speed of component A and the moving speed of component C. By doing so, as shown in the figure, the component A is in front of the raw material supply position as viewed in the flow direction of the eluent, and the component C is behind the raw material supply position, as shown in the figure. Can be taken out with. This method is difficult to use industrially due to the difficulty of moving the filler uniformly.
[0005]
A pseudo moving bed type separation apparatus that can obtain separation performance equivalent to that of the moving bed type without moving the filler has been put into practical use. FIG. 6 shows the principle of this separation apparatus. In this method, the separation tower 50 is divided into a plurality of (in the example shown in the figure, 12) columns 54 and connected endlessly. Instead of the movement of the filler, the supply position of the raw material liquid F and the eluent D and the extraction position of the components A and C are moved in the eluent flow direction. Thereby, with the passage of time, the distribution of the liquid in the system moves in the flow direction of the circulating liquid. After the concentration distribution has moved by one column after a lapse of a fixed time, the supply position of the raw material liquid and the eluent and the extraction position of components A and C are moved by one column in the direction of the circulating liquid flow. By repeating this operation, it is possible to always supply and withdraw liquids at optimum positions.
[0006]
In order to move the circulating fluid supply position and the extraction position, generally, a method of sequentially switching valves is used. For this switching, an individual valve system using four individual valves for each column (for example, Japanese Patent Laid-Open No. 4-334504) and a rotation for controlling the entire column flow by switching with one rotary valve. There is a valve system (for example, JP-A-8-323104). The rotary valve system has been widely used in recent years because the piping configuration and control are simplified.
[0007]
[Problems to be solved by the invention]
In the rotary valve method, generally, a method of rotating a circulation flow path including a column is used. However, a flow path including a large number of columns is heavy, and there are structural problems associated with constantly rotating the flow path. In addition, there is a method of fixing the circulation flow path using a complicated rotary valve or rotary joint (JP-A-8-323104). However, the structure of the rotary valve or rotary joint itself is complicated, so that the manufacturing cost is low. In addition to being bulky, there are drawbacks such as complicated maintenance of the apparatus or problems with the reliability of the apparatus.
[0008]
In view of the above, the present invention provides a simulated moving bed type chromatographic separation device having a rotary valve with a simple structure and low cost, thereby reducing the cost of the simulated moving bed type chromatographic separation device and reducing the size of the device, The purpose is to simplify maintenance and improve reliability.
[0009]
[Means for Solving the Problems]
In order to achieve the above object, the simulated moving bed chromatographic separation apparatus of the present invention comprises at least four columns each having an inlet and an outlet,
An eluent flow path for supplying the eluent, a first extraction flow path for extracting the first component in the raw material liquid containing at least two components, and a second extraction flow for extracting the second component in the raw material liquid Flexible piping including at least a path;
A fixing part having a cylindrical or conical fixing surface, a fixing channel disposed corresponding to each column, a rotating surface that rotates while swinging on the fixing surface, and each of the flexibility A rotary valve having a rotary part having a rotary flow path arranged corresponding to the pipe,
Each fixed flow path communicates with each other, a first nozzle exposed on the fixed surface, a second nozzle communicated with an outlet of one column, and a first nozzle communicated with an inlet of a column adjacent to the one column. Having three nozzles, and connecting the column endlessly as a whole by the fixed flow path,
One end of each of the rotating channels is exposed to the rotating surface and periodically communicates with the first nozzle of the fixed channel, and the other end is connected to the corresponding flexible pipe. And
[0010]
According to the simulated moving bed chromatographic separation apparatus of the present invention, the configuration of the rotary valve is simplified, so that the cost of the entire apparatus can be reduced, the apparatus can be reduced in size, the maintenance can be simplified, and the reliability can be improved.
[0011]
There is no particular limitation on the material of the rotary valve used in the present invention, but for smooth peristalsis on the sliding surface of the rotating part and the fixed part, either the rotating part or the fixed part is made of Teflon resin or polyethylene. It is preferable to manufacture with resin. In this case, the other is made of stainless steel or the like. As the flexible tube, a nylon tube, a Teflon tube, a PEEK tube, a stainless steel tube or the like is preferably used.
[0012]
In a preferred configuration of the present invention, it further includes a raw material liquid channel for supplying the raw material liquid and the rotating flow channel corresponding to the raw material liquid channel, and the raw material liquid channel is further configured as the flexible pipe. . This configuration can be suitably used for a chromatographic separation apparatus in which a raw material liquid containing two components is continuously supplied and the raw material liquid is separated into each component. For example, in the case of a chromatographic separation apparatus in which a raw material liquid containing three components is separated into each component, it is sufficient if there is a raw material liquid flow path for supplying the raw material liquid into the circulation path once in one cycle of the separation step. The raw material liquid channel can be configured as a fixed pipe.
[0013]
It is also a preferred aspect of the present invention that a branching portion that branches from the first nozzle of the fixed flow path to the second nozzle and the third nozzle is disposed adjacent to the first nozzle. This prevents mixing of circulating fluids having different components that occur when the flow path is switched by the rotation of the rotating part.
[0014]
It is also a preferred aspect of the present invention that the rotating portion reverses when the rotation angle reaches a preset angle and returns to a predetermined rotation angle position. Thereby, since the rotation angle of the rotating part can be limited to, for example, 360 ° or less, twisting of the flexible piping can be minimized, and a stainless tube or the like can be suitably used as the flexible piping.
[0015]
DETAILED DESCRIPTION OF THE INVENTION
With reference to the drawings, the present invention will be described in more detail based on a simulated moving bed type chromatographic separation apparatus (hereinafter simply referred to as a chromatographic separation apparatus) according to an embodiment of the present invention.
[0016]
FIG. 1 is a schematic perspective view showing the overall configuration of a chromatographic separation apparatus according to an embodiment of the present invention. The chromatographic separation apparatus includes a rotary valve 10, and the rotary valve 10 has a substantially frustum-shaped rotary part (rotary body) 30 disposed radially inward, and a cone that is in sliding contact with the conical surface of the rotary body 30. It is comprised with the fixed part 32 which has a trapezoid internal peripheral surface and a substantially cylindrical external shape. The rotating body 30 has four rotating flow paths formed therein, and the four rotating flow paths are configured as a flexible pipe 44 and a raw material liquid tube for supplying a raw material liquid containing the component A and the component C. And an eluent supply tube for supplying the eluent, a first extraction tube for extracting the separation component A, and a second extraction tube for extracting the separation component C, respectively. The thickness of the flexible tube 44 is, for example, about 1 to 5 mm.
[0017]
Eight columns 20 are arranged on the outer fixed portion 32 of the rotary valve 10 at substantially equal intervals in the circumferential direction adjacent to the outer side in the radial direction. The eight columns 20 are connected in an endless ring shape through a fixed flow path in the fixed portion 32 of the piping 22, the check valve 34, and the rotary valve 10. The column size is, for example, about 10 to 50 cm in length and about 1 to 10 cm in diameter. The rotating body 30 of the rotary valve 10 corresponds to the moving speed of the circulating fluid moving in the system, and is rotated counterclockwise on the drawing by the stepping motor 24. This rotation is an intermittent rotation that rotates by 1/8 of one revolution in one operation, and for example, moves one notch at intervals of 5 minutes and makes one revolution in about 40 minutes. In this case, the rotator 30 reverses and returns to the initial angular position after 7/8 rounds from the initial angular position. In the circulation path connecting the columns 20, one or more circulation pumps (not shown) are arranged at appropriate positions.
[0018]
The rotation angle of the rotating body 30 is detected by a photo interrupter 26 and a holed disk 28 for detecting the rotation angle position. The photo interrupter 26 reverses the stepping motor 24 by a predetermined angle immediately after detecting the light transmitted through the hole. The rotating body 30 is returned to the initial angular position.
[0019]
FIG. 2 shows a connection relationship between the rotating unit 30 of the rotary valve 10 and each raw material tank and separated product tank. The chromatographic separation apparatus includes a two-component raw material liquid tank 12, an eluent tank 14, an A component tank 16, and a C component tank 18. These tanks are connected to a raw material liquid supply port F, an eluent supply port D, a component A extraction port A, and a component C extraction port C of the rotating unit 30, respectively, a fixed pipe 42, a pump 40, and a flexible tube. 44 is connected. The raw material liquid only needs to contain two or more components, and may contain three or more components.
[0020]
FIG. 3 is a schematic view including a cross section of the rotary valve 10 showing a connection relationship between the fixed portion 32 of the rotary valve 10 and each column 20. A flow path (fixed flow path) 38 connected to the pipe 22 from each column 20 is formed in the fixed portion 32 corresponding to each column. Each fixed flow path 38 has a first nozzle exposed on the inner fixed surface of the fixed portion 32, and second and third nozzles respectively connected to the outlet and inlet of the column 20 adjacent to each other. The nozzles communicate with each other in a Y shape in the vicinity of the conical inner surface (fixed surface) of the fixed portion 32 in each fixed flow path. Each Y-shaped communication portion is arranged at a predetermined rotation angle position in sequence in the rotation direction of the rotator 30, the raw material liquid supply port F, the component A extraction port A, and the eluent. It communicates with a flow path (rotary flow path) 36 in the rotating body 30 connected to the supply port D and the component C extraction port C. A check valve 34 for restricting the flow of the circulating fluid in the counterclockwise direction that is the rotational direction of the rotating body 30 is disposed in the middle of the pipe 22 that connects each column 20 and the fixed portion 32.
[0021]
FIG. 4 is a side view showing a part of the structure of the rotary valve 10 in a longitudinal section. The rotary valve 10 includes an inner rotary body 30 and an outer fixed portion 32, and the rotary body 30 is driven by a stepping motor via a shaft 46. The rotating body 30 as a whole has a truncated cone shape whose lower surface is smaller than the upper surface. The fixed portion 32 has a substantially cylindrical outer peripheral surface with a slightly smaller radius at the bottom, and the inner peripheral surface has a truncated cone shape that is in contact with the conical surface of the rotating body 30. A rotating flow path 36 corresponding to each tank is formed inside the rotating body 30, and the rotating flow path 36 is disposed in an L shape between the conical surface and the lower surface of the rotating body 30. The end of the rotary channel 36 on the lower side of the truncated cone is connected to the flexible tube 44 via the joint 48 and communicates with each tank via the flexible tube 44 as described above.
[0022]
The end of the rotary channel 36 on the side of the truncated cone is in communication with the first nozzle of the fixed channel 38 on the fixed part 32 side at the rotational angle position shown in the figure. One branch of the fixed channel 38 extending in the lateral direction from the first nozzle communicates with the outlet of the corresponding column 20 via the second nozzle, and constitutes an inlet channel through which the circulating fluid flows from the column 20. To do. Further, the other branch extending obliquely downward from the first nozzle communicates with the inlet of the adjacent column 20 on the downstream side via the third nozzle, and an outlet channel through which the circulating fluid flows out to the column 20 is provided. Constitute. Each branch extends substantially orthogonally to the outer surface of the fixed portion 32, so that the manufacturing convenience when machining by cutting or the like is achieved.
[0023]
As described above, the flexible tube 44 is connected to the rotary valve 30. Here, when the rotating body 30 is intermittently rotated in the counterclockwise direction and the total rotation angle reaches approximately 360 ° from the original position, the flexible tube 44 is not a little twisted. However, this twist is eliminated by the next reverse rotation in which the rotating unit 30 returns to the original position. As described above, in the chromatographic separation apparatus according to the present embodiment, the flexible tube 44 is used for connection between the rotating body 30 of the rotary valve 10 and each tank, so that the connection between the rotary valve 10 and the column 20 is fixed piping. 22 and there is an advantage that the apparatus configuration is simplified. As the flexible tube 44, a tube made of plastic or stainless steel can be used. Here, in order to absorb the twist effectively, the flexible tube 44 is processed into a spiral shape.
[0024]
The fixed portion 32 of the rotary valve 10 is made of, for example, a corrosion-resistant stainless material, and the rotating body 30 is preferably made of Teflon resin or polyethylene resin having lubricity. Alternatively, the rotating body 30 may be made of stainless steel, and the fixed portion 32 may be made of Teflon resin or polyethylene resin having lubricity.
[0025]
The chromatographic separation apparatus of this embodiment operates in the same manner as the conventional simulated moving bed type chromatographic separation apparatus having a rotary valve, and supplies the raw material liquid and the eluent from the raw material supply port F and the eluent supply port D, respectively. By rotating the rotary valve according to the moving speed of the circulating fluid, the components A and C are extracted from the A and C outlets, respectively.
[0026]
As mentioned above, although this invention was demonstrated based on the suitable embodiment example, the simulated moving bed type | formula chromatographic separation apparatus of this invention is not limited only to the structure of the said embodiment example, The said embodiment example is not limited. Pseudo moving bed chromatographic fractionation devices having various modifications and changes in configuration are also included in the scope of the present invention.
[0027]
【The invention's effect】
As described above, according to the simulated moving bed type chromatographic separation apparatus of the present invention, the column connected in an endless manner is connected to the fixed portion of the rotary valve. The structure is simplified and the maintenance work becomes easy. Further, since the number of parts in the vicinity of the rotary valve can be reduced and the piping structure can be simplified without complicating the structure of the rotary valve, the manufacturing cost of the chromatographic separation apparatus can be reduced.
[Brief description of the drawings]
FIG. 1 is a schematic perspective view showing the configuration of a simulated moving bed chromatographic separation apparatus according to an embodiment of the present invention.
FIG. 2 is a block diagram of piping that connects a rotary part of a rotary valve of the chromatographic separation apparatus of FIG. 1 and each tank.
3 is a schematic view including a cross section of a rotary valve, showing a connection between a fixed portion of the chromatographic separation apparatus of FIG. 1 and each column.
4 is a longitudinal sectional view of the rotary valve shown in FIG.
FIG. 5 is a schematic sectional view of a separation tower showing the principle of a general moving bed chromatographic separation apparatus.
FIG. 6 is a schematic cross-sectional view of a separation tower showing the principle of a general pseudo moving bed type chromatographic separation apparatus.
[Explanation of symbols]
10: Rotating valves 12, 14, 16, 18: Tank 20: Column 22: Circulating piping 24: Stepping motor 26: Photo interrupter 28: Perforated disk 30: Rotating body (rotating part)
32: Fixed part 34: Check valve 36: Rotating flow path 38: Fixed flow path 40: Pump 42: Pipe 44: Flexible pipe 46: Shaft 48: Fitting

Claims (5)

At least four columns each having an inlet and an outlet;
An eluent flow path for supplying the eluent, a first extraction flow path for extracting the first component in the raw material liquid containing at least two components, and a second extraction flow for extracting the second component in the raw material liquid Flexible piping including at least a path;
A fixing part having a cylindrical or conical fixing surface, a fixing channel disposed corresponding to each column, a rotating surface that rotates while swinging on the fixing surface, and each of the flexibility A rotary valve having a rotary part having a rotary flow path arranged corresponding to the pipe,
Each fixed flow path communicates with each other, a first nozzle exposed on the fixed surface, a second nozzle communicated with an outlet of one column, and a first nozzle communicated with an inlet of a column adjacent to the one column. Having three nozzles, and connecting the column endlessly as a whole by the fixed flow path,
One end of each of the rotating channels is exposed to the rotating surface and periodically communicates with the first nozzle of the fixed channel, and the other end is connected to the corresponding flexible pipe. A pseudo moving bed type chromatographic separation apparatus. 2. The simulated moving bed chromatographic separation device according to claim 1, wherein a branching portion that branches from the first nozzle into the second nozzle and the third nozzle is disposed adjacent to the first nozzle. The pseudo moving bed type chromatographic separation apparatus according to claim 1, wherein the flexible pipe has flexibility corresponding to a predetermined rotation angle of the rotating unit. 3. The simulated moving bed chromatographic separation device according to claim 1, wherein the rotation unit reverses and returns to a predetermined rotation angle position when a total rotation angle reaches a preset angle. The raw material liquid flow path for supplying the raw material liquid and the rotating flow path corresponding to the raw material liquid flow path are further included, and the raw material liquid flow path is further configured as the flexible pipe. The simulated moving bed type chromatographic separation apparatus according to any one of the above.

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