JP2000162198A - Pseudo moving bed type chromatographic separating device - Google Patents

Abstract

PROBLEM TO BE SOLVED: To suppress the pressure distribution and pressure fluctuation in the circulating passage of a pseudo moving bed type chromatographic separating device to suppress the concentration fluctuation of a circulating solution and to provide a desired separating performance. SOLUTION: This device has a circulating passage having separation columns endlessly connected thereto, so that a binary system raw material solution and an eluent are injected from tanks 12, 14, and separated components A and C are extracted to tanks 16, 18. As each of first and second circulating pumps 52, 56 for circulating the solution, a raw material solution injection pump 54 and an eluent injection pump 58, a 1-cylinder type plunger pump is used. The plungers of the first circulating pump 52 and the second circulating pump 56, and the plungers of the raw material solution injection pump 56 and the eluent injection pump 58 are set so as to have mutually reverse phases, respectively, and all the pumps are synchronously driven, whereby the pressure distribution and pressure fluctuation within the system are suppressed to prevent the fluctuation of the concentration distribution.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a simulated moving bed type chromatographic separation apparatus, and more particularly, to control of a pump in a simulated moving bed type chromatographic separation apparatus.

[0002]

2. Description of the Related Art Chromatographic separation apparatuses are widely used in the manufacturing industry, such as the sugar industry and the pharmaceutical industry, for the purpose of extracting one or more components from a raw material fluid composed of a plurality of components obtained by natural or chemical reactions. I have. Various types of chromatographic separation apparatuses have recently been proposed in addition to the conventionally used batch fixed bed system, and recently a moving bed system.

FIG. 4 is a schematic sectional view of a separation column showing the principle of a moving bed type chromatographic separation apparatus. The separation tower 70 is filled in advance with a filler (adsorbent) 72, which is 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 the eluent supply port D so as to have a constant linear velocity. Each component A and C
Moves at different linear velocities in the separation tower 70 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 moves at a low linear velocity. Therefore, it can be separated into a fraction containing a large amount of component A and a fraction containing a large amount of component C.

In the moving bed type chromatographic separation apparatus, a state is created in which the packing material is moved in the direction opposite to the flow of the eluent at a speed intermediate between the moving speed of the component A and the moving speed of the component C. By doing so, as shown in the drawing, the component A is located in front of the raw material supply position and the component C is located behind the raw material supply position when viewed in the flow direction of the circulating liquid. Can be taken out. This method has a difficulty in practically industrially using it because of the difficulty in moving the filler uniformly.

[0005] A simulated moving bed type separation apparatus capable of obtaining the same separation performance as a moving bed type without moving a filler has been put into practical use. FIG. 5 shows the principle of this separation device. In this method, the separation tower 70 is divided into a plurality of (twelve in the example in the figure) columns 74, which are connected endlessly. Instead of moving 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 flow direction of the eluent. As a result, the distribution of the liquid in the system moves in the flow direction of the circulating liquid over time.
After a certain period of time, after the concentration distribution moves by one column, the supply position of the raw material liquid and the eluent and the extraction position of the components A and C are moved by one column in the flow direction of the circulating liquid. By repeating this operation, it is possible to always supply and withdraw each liquid at an optimum position.

For driving the circulating liquid, a driving force of a circulating pump disposed in a circulation path is used in addition to a driving force of a raw material liquid injection pump and an eluent injection pump. Each pump is a non-pulsating reciprocating pump (hereinafter simply referred to as a non-pulsating pump) in order to minimize pressure fluctuations in the system.
Is used. The non-pulsation pump is provided with a plurality of plungers (pistons), and has a phase difference in the movement of each plunger to compensate for fluctuations in the discharge flow rate during one rotation of the crankshaft. Used for

[0007]

When the circulating fluid is driven by the circulating pump, a pressure distribution occurs in the system due to the arrangement of the circulating pump. Although this pressure distribution can be eliminated by arranging a plurality of circulation pumps at appropriate positions in the circulation path, providing a plurality of expensive non-pulsation pumps increases the cost of the simulated moving bed type chromatograph. Become a factor.

Here, for example, as a plurality of circulation pumps,
When a normal reciprocating pump is used in place of a non-pulsating pump in a simulated moving bed type chromatographic separation apparatus, a large pressure fluctuation occurs in the system, so that the concentration distribution in the system cannot be maintained at the design value, and the desired separation Performance cannot be obtained.

In view of the above, the present invention provides a simulated moving bed type chromatographic separation apparatus capable of preventing a non-uniform flow rate distribution and a concentration distribution caused by pressure distribution and pressure fluctuation in a system and reducing costs. With the goal.

[0010]

In order to achieve the above object, a simulated moving bed type chromatographic separation apparatus of the present invention comprises at least four columns having an inlet and an outlet, and connects the inlet and the outlet of the columns. An endless circuit, a material liquid injection pipe for injecting a material liquid containing at least two components into a first predetermined position in the circuit, and an eluent in a second predetermined position in the circuit. An eluent injection pipe for injecting, a circulation pump for supplying a liquid stream at a predetermined speed to the raw material liquid and the eluent in the circulation path, and a third and a fourth predetermined position in the circulation path, respectively, connected to the third And a pair of extraction pipes for separating and extracting the two components from a fourth predetermined position, respectively, wherein the circulation pump is associated with a position in the circulation path that is separated from each other in the circulation path. First and second The circulation pump, the first and second circulation pump, characterized by being composed of a pair of one-cylinder plunger pump or a diaphragm pump to operate synchronously each other in opposite phases.

According to the simulated moving bed type chromatographic separation apparatus of the present invention, while using an inexpensive one-cylinder type plunger pump or diaphragm pump as the circulation pump, the pressure fluctuation is suppressed by reducing the volume fluctuation in the circulation path system. Fluctuations can be suppressed, and fluctuations in the concentration distribution can also be suppressed, so that desired separation performance can be obtained.

In a preferred aspect of the present invention, a first check valve for restricting the liquid flow of the raw material liquid in one direction is provided in the raw material liquid injection pipe, and the discharge port of the first circulation pump is connected to the first reverse pump. A second check valve connected between the stop valve and the first predetermined position, and a second check valve for restricting the flow of the eluent in one direction in the eluent injection pipe;
Is connected between the second check valve and the second predetermined position. In this case, it is possible to suppress the influence of the stirring action generated in the cylinder of the pump on the separation performance.

In the raw material liquid injection pipe, a third check valve is provided at a position farther from the first predetermined position than the first check valve in the same direction as the liquid flow direction of the first check valve. A raw material liquid injection pump having a discharge port connected between the first check valve and the third check valve; and a second predetermined position in the eluate liquid injection pipe. A fourth check valve is disposed on a side farther than the second check valve in the same direction as the liquid flow direction of the second check valve.
It is also a preferred embodiment of the present invention that an eluent injection pump having a discharge port connected to the check valve is provided and the raw material injection pump and the eluent injection pump are synchronously operated in opposite phases.
In this case, a circulating liquid flow having a stable flow distribution can be obtained.

It is also preferable to insert a back pressure valve, which opens when the pressure at the third and fourth predetermined positions rises above a predetermined value, into each of the pair of extraction tubes. In this case, since the extraction pump can be omitted, the device configuration is simplified.

[0015]

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS The present invention will be described in more detail with reference to the drawings based on a simulated moving bed type chromatograph (hereinafter simply referred to as chromatograph) of one embodiment of the present invention.

FIG. 1 is a schematic perspective view showing the overall structure of a chromatographic separation apparatus according to one embodiment of the present invention. The chromatographic separation apparatus has a rotary valve 10, and the rotary valve 10 is a rotary unit (rotator) having a substantially frustoconical shape disposed radially inward.
And a fixed portion 32 having a truncated cone-shaped inner peripheral surface and a substantially cylindrical outer shape that are in sliding contact with the conical surface of the rotating body 30. Four rotating flow paths are formed inside the rotating body 30, and the four rotating flow paths include a raw material liquid tube configured as a flexible pipe 44 and configured to supply a raw material liquid containing the components A and C. , An eluent supply tube for supplying an eluent, a first extraction tube for extracting the separation component A, and a second extraction tube for extracting the separation component C.

The raw material tube has two check valves 48A,
The eluent tube is connected to the raw material tank 12 via a fixed pipe 46 into which the 48B is inserted.
8C and 48D are connected to the eluent tank 14 via a fixed pipe 46 into which the eluent is inserted. The component A extraction tube and the component C extraction tube are back pressure valves 60A and 60B, respectively.
Are connected to the separation component A tank 16 and the separation component C tank 18 via the fixed piping 46 into which the is inserted.

Eight columns 20 are arranged on the outer fixed portion 32 of the rotary valve 10 adjacent to the outer side in the radial direction at substantially equal intervals in the circumferential direction. Eight columns 20 are connected to pipe 2
2. It is connected in an endless annular shape through a check valve 34 and a fixed flow path in the fixed portion 32 of the rotary valve 10. Each column is filled with a packing material. The size of the column 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 is rotated counterclockwise on the drawing by the stepping motor 24. This rotation is an intermittent rotation that rotates by 1/8 of one rotation in one operation.
Make one lap in about a minute. In this case, the rotating body 30 reverses and returns to the initial angular position after 7/8 rotation from the initial angular position.

The rotation angle of the rotator 30 is detected by a photo interrupter 26 for detecting the position of the rotation angle and a perforated disk 28. The photo interrupter 26 immediately turns the stepping motor 24 by a predetermined angle upon detecting the light transmitted through the hole. Then, the rotating body 30 is returned to the initial angular position.

FIG. 2 is a schematic diagram including the cross section of the rotary valve 10 showing the configuration of the rotary valve 10 and the connection relationship thereof. In the fixing part 32, a flow path (fixed flow path) 38 connected to the pipe 22 from each column 20 is formed corresponding to each column 20. Two nozzles connected to the inlet and outlet of the column 20 which are adjacent to each other are connected to a fixed portion 32 in a fixed flow path.
In a Y-shape near the conical inner surface. Each Y
The letter-shaped communicating portion is provided at a predetermined rotation angle position with a supply port F for a raw material liquid, a discharge port A for a component A, and a supply port D for an eluent, which are sequentially arranged in the rotation direction of the rotating body 30. And, it communicates with a flow path (rotation flow path) 36 in the rotating body 30 connected to the outlet C of the component C. Each column 20 and fixed part 3
A check valve 34 for restricting the flow of the circulating liquid in the counterclockwise direction, which is the direction of rotation of the rotating body 30, is provided in the middle of the pipe 22 connecting the first and second pipes.

FIG. 3 shows the connection relationship between the rotating body 30 of the rotary valve 10 and each of the tanks 12, 14, 16, and 18 and the configuration of each pump. In the present chromatographic separation apparatus, the two-component raw material liquid tank 12, the eluent tank 14, the A-component tank 16, and the C-component tank 18 are respectively provided with the raw material liquid supply port F and the eluent supply port D of the rotating body 30. , Component A outlet A,
And, it is connected to the component C outlet C via a fixed pipe 46 and a flexible tube 44, respectively. The raw material liquid only needs to contain two or more components, and may contain three or more components.

In the middle of the fixed pipe 46 connecting the raw material liquid tank 12 and the flexible tube 44, two check valves 48
A and 48B are inserted in the same direction and in a direction allowing only the liquid flow from the raw material liquid tank 12. Between the flexible tube 44 and the first check valve 48A, a cylinder chamber (discharge port) of a first circulating pump 52 configured as a one-cylinder type plunger pump is connected, and a first reverse valve is provided. Between the stop valve 48A and the third check valve 48B, a cylinder chamber of a raw material liquid injection pump 54 also configured as a one-cylinder type plunger pump is connected.

In the middle of the fixed pipe 46 connecting the eluent tank 14 and the flexible tube 44, two check valves 48
C and 48D are inserted in the same direction and in a direction that allows only the liquid flow from the eluent tank 14. Between the flexible tube 44 and the second check valve 48C, a cylinder chamber of a second circulating pump 56 configured as a one-cylinder type plunger pump is connected, and the second check valve 48C and the second check valve 48C are connected to each other. Between the fourth check valve 48D and the fourth check valve 48D, an eluent injection pump 5 also configured as a one-cylinder type plunger pump
8 cylinder chambers are connected.

A back pressure valve 60A is inserted between the A component tank 16 and the flexible tube 44. The back pressure valve 60A
When the pressure on the circulation path side rises to a predetermined value or more, it is opened, and the separation component A is extracted from the circulation path to the tank 16. That is, the back pressure valve 60A allows only the liquid flow of the component A toward the tank. Similarly, a back pressure valve 60B is inserted between the C component tank 18 and the flexible tube 44, and the back pressure valve 60B allows only a liquid flow toward the separated component C tank.

Each plunger of the first circulation pump 52, the raw material liquid injection pump 54, the second circulation pump 56, and the eluent injection pump 58 is driven by a crank 66 which is rotatably supported by a common crankshaft 68. You. The crankshaft 68 is supported at two places by a bearing 64 and is driven by the pump drive motor 50 via the coupling 62 at one end. The pump capacity of the first circulation pump 52 and the second circulation pump 56 are substantially the same, and the pump capacity of the raw material liquid injection pump 54 and the eluent injection pump 58 are also substantially the same. here,
As shown, when each plunger of the first circulation pump 52 and the raw material liquid injection pump 54 is at the bottom dead center, each plunger of the second circulation pump 56 and the eluent injection pump 58 is at the top dead center. Then, each pump is driven synchronously.

That is, the first circulation pump 52 and the raw material liquid injection pump 54 are always driven synchronously. In this synchronization, it is not necessary to synchronize in phase such that both plungers are at top dead center or bottom dead center at the same time, for example, so that both plungers are in phase or opposite phase, or in a fixed phase relationship. Driven to keep. Similarly, the second circulation pump 56 and the eluent injection pump 58 are driven synchronously so as to maintain a constant phase relationship. Further, the first circulating pump 52 and the second circulating pump 56 are synchronously driven so as to have mutually opposite phases, and the raw material liquid injection pump 54 and the eluent injection pump 58 have mutually opposite phases. Are driven synchronously so that

In FIG. 3, when the pump drive motor 50 is operated, each pump is driven by a corresponding crank 66. For example, when the plunger of the first circulating pump 52 moves from the bottom dead center to the top dead center in the drawing, the volume in the system decreases accordingly, and the pressure in the system increases. The pressure increase is caused by the fixed pipe 46, the flexible tube 44, the raw material liquid supply port F of the rotary body 30 of the rotary valve 10, the corresponding rotary flow path 36 in the rotary body 30, and the fixed portion communicating therewith. 3
The fluid is transmitted via the column 20 located in the forward path defined by the second fixed flow path 38 and the check valve 34.
This transmitted pressure rise is absorbed by the movement of the second circulation pump 56 from the top dead center to the bottom dead center.

That is, the pressure increase in the circulation flow path by the first circulation pump 52 is caused by the fixed flow path 38 disposed opposite to the fixed flow path 38 connected to the raw material supply port F at that time, and
It is absorbed by the movement of the plunger from the top dead center to the bottom dead center of the second circulating pump 56 via the eluent supply port D communicating therewith. For this reason, the pressure in the circulation path system does not substantially increase. Similarly, the pressure drop due to the movement of the first circulation pump 52 from the top dead center to the bottom dead center of the plunger is absorbed by the movement of the second circulation pump 56 from the bottom dead center to the top dead center. That is, the first and second circulation pumps are operated synchronously while minimizing pressure fluctuations in the system.

Most of the liquid in the cylinder discharged by the in-phase operation of the raw material liquid injection pump 54 and the plunger of the first circulation pump 52 enters the cylinder of the second circulation pump 56 which operates synchronously. The suction is performed, and the remaining part gives a slight pressure rise in the system, and opens the back pressure valve 60A disposed in the forward path of the circulation path. Thereby, the separation component A is extracted into the tank 16. Most of the liquid discharged by operating the eluent injection pump 58 and the plunger of the second circulation pump 56 in the same phase is the first circulation pump 5
2, the remaining part gives a slight pressure rise in the system, and opens the back pressure valve 60B disposed in the forward path of the circulation path. Thereby, the separation component C is extracted to the tank 18.

The chromatographic separation apparatus of this embodiment is shown in FIG.
The separation operation is performed in the same manner as in the conventional simulated moving bed type chromatographic separation apparatus whose principle is shown in FIG. That is, by driving the pump drive motor 50, the raw material liquid injection pump 54 and the eluent injection pump 58 are operated, and the raw material liquid is supplied from the tanks 12 and 14 via the raw material supply port F and the eluent supply port D, respectively. And an eluent are supplied. At the same time, the first and second circulation pumps 52 and 56 operate to create a circulating fluid flow in the circulation path. When the rotary valve 10 is rotated according to the moving speed of the circulating liquid, the component A and the component C are separated. Back pressure valves 60A, 60B disposed at positions where the pressure in the circulation path has increased
Are opened, and components A and C are respectively discharged from the liquid outlet of the circulation path.
Is drawn out to the tanks 16 and 18. In the rotation of the rotary valve 10, the rotary body 30 of the rotary valve 10 is intermittently moved by one notch in a counterclockwise direction according to the moving speed of the circulating fluid. When the total rotation angle reaches approximately 360 ° from the original position, a considerable amount of twist occurs in the flexible tube 44, but this twist is eliminated by the next reverse rotation of the rotating unit 30 returning to the original position.

In the simulated moving bed type chromatograph of the above embodiment, the pressure distribution in the system is reduced by employing a pair of one-cylinder type plunger pumps spaced apart from each other in the circulation path. Since the pressure distribution becomes uniform and the pressure hardly fluctuates, the fluctuation of the concentration distribution in the circulation channel can be prevented, and the desired separation performance can be obtained.

In the above embodiment, an example of a simulated moving bed type chromatograph having eight columns 20 has been described, but the number of the columns 20 is four or more, preferably
Multiples of four are provided.

In the above embodiment, an example of a simulated moving bed type chromatograph using a rotary valve has been described. However, the simulated moving bed type chromatograph of the present invention is not necessarily a rotary valve type. The present invention is not limited to this, and may be applied to a simulated moving bed type chromatographic separation apparatus of an individual valve type in which a valve is individually arranged in each column instead of the rotary valve type.

As described above, the present invention has been described in detail based on the preferred embodiments. However, the present invention is not limited to only the configuration of the above-described embodiment, and various modifications may be made from the configuration of the above-described embodiment. Modifications and changes are also included in the scope of the present invention.

[0035]

As described above, according to the simulated moving bed type chromatographic separator of the present invention, the use of a pair of one-cylinder type plunger pumps or diaphragm pumps allows the pressure distribution and the pressure distribution in the circulation flow path to be improved. Pressure fluctuation can be suppressed, and desired separation performance can be obtained. Therefore, there is an effect that the production cost can be reduced while maintaining the performance of the simulated moving bed type chromatographic separation apparatus at a high level.

[Brief description of the drawings]

FIG. 1 is a schematic perspective view showing a configuration of a simulated moving bed type chromatographic separation apparatus according to an embodiment of the present invention.

FIG. 2 is a schematic view showing the configuration and connection of the rotary valve, including a cross section of the rotary valve.

FIG. 3 is a system diagram showing a connection between a rotating part of a rotary valve, a column, and a tank.

FIG. 4 is a schematic sectional view of a separation tower showing the principle of a general moving bed type chromatographic separation apparatus.

FIG. 5 is a schematic sectional view of a separation tower showing the principle of a general simulated moving bed type chromatographic separation apparatus.

[Explanation of symbols]

 10: Rotary valve 12, 14, 16, 18: Tank 20: Column 22: Circulation pipe 24: Stepping motor 26: Photo interrupter 28: Perforated disk 30: Rotating body (rotating part) 32: Fixed part 34: Non-return Valve 36: Rotating flow path 38: Fixed flow path 44: Flexible tube 46: Fixed piping 48A, 48B, 48C, 48D: Check valve 50: Pump drive motor 52: First circulation pump 54: Raw material liquid injection pump 56: second circulation pump 58: eluent injection pump 60A, 60B: back pressure valve 62: coupling 64: bearing 66: crank 68: crankshaft

Continued on the front page (51) Int.Cl. ⁷ Identification symbol FI Theme coat II (Reference) G01N 30/46 G01N 30/46 A 30/60 30/60 B (72) Inventor Takayuki Masuda 1-chome Shinsuna, Koto-ku, Tokyo No.2 Organo Co., Ltd. (72) Inventor Kohei Sato 1-2-8 Shinsuna, Koto-ku, Tokyo Organo Co., Ltd. (72) Inventor Manabu Yasuda 1-2-8 Shinsuna, Koto-ku, Tokyo Organo Corporation F term (reference) 3H071 AA01 BB01 BB12 CC17 CC25 CC34 CC37 CC47 DD12 DD13 DD14 DD17 DD31 DD42 4D017 AA03 AA07 BA03 DA02 DA03 EA01 EB10

Claims (4)

[Claims] 1. An endless circuit formed by connecting at least four columns having an inlet and an outlet with the inlet and the outlet of the column, and at least two components in a first predetermined position in the circuit. An eluent injection pipe for injecting an eluent into the second predetermined position in the circulation path, and a liquid flow at a predetermined speed to the eluent and the eluent in the circulation path. And a third pump of the circulation path
A simulated moving bed type chromatographic separation apparatus comprising: a pair of extraction pipes respectively connected to a fourth predetermined position and a second extraction pipe for separating and extracting the two components from the third and fourth predetermined positions, respectively. Are first and second circulating pumps disposed in relation to mutually separated positions in the circulation path, and a pair of the first and second circulating pumps that operate synchronously in opposite phases to each other. A simulated moving bed type chromatograph separating apparatus comprising a one-cylinder plunger pump or a diaphragm pump. 2. A first check valve for regulating a liquid flow of a raw material liquid in one direction is provided in the raw material liquid injection pipe, and a discharge port of the first circulating pump is connected to the first check valve. And the first predetermined position.
A second check valve for regulating the direction is provided, and a discharge port of the second circulation pump is connected between the second check valve and the second predetermined position. A simulated moving bed type chromatographic separation apparatus according to claim 1. 3. A third check valve is provided in the raw material liquid injection pipe at a position farther from the first predetermined position than the first check valve, and a liquid flow direction of the first check valve is provided. And a raw material liquid injection pump having a discharge port connected between the first check valve and the third check valve. A fourth check valve is disposed on the side farther than the second check valve from the predetermined position of the second check valve in the same direction as the liquid flow direction of the second check valve; An eluent injection pump having a discharge port connected between the eluent injection pump and the fourth check valve, wherein the raw material liquid injection pump and the eluent injection pump are synchronously operated in opposite phases. ,
A simulated moving bed type chromatographic separation apparatus according to claim 2. 4. The method according to claim 1, wherein each of the pair of extraction tubes is provided with a third one.
The simulated moving bed type chromatographic separation apparatus according to any one of claims 1 to 3, wherein a back pressure valve that opens when the fourth pressure rises is inserted.