JPH04143658A - Chromatography separation method and simplified pseudo traveling layer device - Google Patents

Abstract

PURPOSE:To achieve utilization efficiency and separation performance with a high filling agent and enable load of complexity in control to be reduced by performing a first process for extracting a fraction where constituents are enrich and a second process for forming a band where each constituent is enrich repeatedly. CONSTITUTION:In a first process, a screen valve is closed, a desorption agent fluid D is supplied to a filling layer 1 from an upstream edge, and a fraction of B constituent with a strong hydrophilic force is extracted to an adsorption agent from a downstream edge. A raw material fluid F is supplied to a filling layer 2 from an upstream edge and a fraction of A constituent with a weak hydrophilic force is extracted from a downstream edge to the adsorption agent. At the end of the first process, a supply valve and an extraction valve are closed, a shut-off valve is opened, and a circulation pump is operated, thus enabling a fluid to be flowed in circulation at the second process until a front edge of the constituent A within a filling layer 2 reaches a downstream edge position of the filling layer 1. Then, a band where only the constituent B is enrich is formed within the filling layer 2. By repeating this process, the constituents A and B which are included in a raw material fluid can be separated easily. Also, by separating the process into two parts, a high utilization efficiency and separation performance of filing agent can be obtained.

Description

Detailed Description of the Invention (Industrial Application Field) The present invention relates to a method and apparatus for chromatographically separating two or more fractions enriched in each component from a mixed fluid containing two or more components. .

(Prior art) A method of chromatographically separating each component from a mixed fluid containing two or more components using a solid adsorbent by utilizing the difference in adsorption characteristics of the adsorbent has been widely used industrially. However, due to the difference in separation methods, for example, JP-A-63-158
The method is broadly divided into a batch method as shown in No. 105, and a pseudo moving bed method in which a large number of packed beds are connected in series for circulation and separation is carried out while a fluid is continuously flowing inside the bed.

The former batch chromatographic separation method has the advantage that, for example, the position at which the raw material fluid is supplied to the fixed bed and the position at which the separated fraction is extracted are fixed, and it can be operated with simple operation. However, on the other hand, since the raw material fluid is only supplied to the equipment from one place,
Only the adsorbent at the location where the raw material fluid is supplied is always in contact with the highly concentrated raw material fluid, and is therefore in a situation where it is easily subjected to physical and chemical shocks, making it difficult to use the adsorbent. There are problems that it is difficult to say that the method is appropriate, and that there are zones in which the components contained in the raw material fluid are enriched for each component, and zones in which each component is mixed in the unseparated process. While the zone moves, the supply of raw material fluid and the extraction position of each fraction are fixed as described above (as they are fixed, the entire packed bed cannot be effectively involved in separation, resulting in poor separation performance. However, if the amount of adsorbent is the same, it has the disadvantage that it is far inferior to a pseudo-moving bed.

On the other hand, in the latter pseudo-moving bed chromatographic separation method described above, for example, four towers of adsorbent layers are connected in series for circulation, and while a raw material fluid containing two components is supplied to the first tower, A unit of operation is to extract a fraction enriched in one component and simultaneously to extract a fraction enriched in another component from the third column while simultaneously supplying an eluent to the third column;
A method in which the feeding position of the raw material fluid and the extraction position of each fraction are intermittently and sequentially shifted to the next column in accordance with the movement of the enriched zone of each component by this operation. It is. In this way, the pseudo moving bed is a separation method that uses the principle of a moving bed, so it has the advantage of high utilization efficiency of the filler (adsorbent) and very good separation performance. , this separation method requires a small number of unit packed beds (four in total), and continuous circulation of the raw material fluid and desorbent fluid (eluent) while continuously circulating the fluid across these multiple packed beds. It is necessary to continuously supply and extract the enriched zone of each component as each fraction, and also to move the position of fluid supply and extraction, making the operation extremely complicated. There is a problem in that control is difficult because the control is performed in accordance with the flow of fluid within the chamber.For this reason, the device configuration is complicated and expensive, as it usually requires a control computer and a large number of various measuring instruments. There is also the problem that it is easy to become

Furthermore, in this pseudo moving bed type chromatographic separation method, changes in the type and concentration of the eluent that are normally carried out in batch type chromatographic separation devices, such as HPLC, which is mainly used for analytical purposes. However, it has the disadvantage that it is very difficult to adopt because it is a continuous operation type.

Therefore, there is also the drawback that the method is limited in its application to separations that do not involve (need to) change the desorbent fluid (eluent).

(Problems to be Solved by the Invention) As described above, the batch method and the pseudo moving bed method, which are conventionally known as chromatographic separation methods that separate each component as a fraction enriched from a raw material fluid containing a plurality of components, are Although each method has issues to be improved, the operations of these methods are based on completely different principles, so the advantages of one method cannot be applied to the other method.

Therefore, the present inventor has developed the present invention based on an operating principle different from the batch type or conventional simulated moving bed type chromatographic separation method (a new simulated moving bed apparatus and chromatographic separation method). This is what led to this.

That is, an object of the present invention is to provide a new romato separation method and a simulated moving bed that can reduce the burden of control complexity in the simulated moving bed apparatus while exhibiting high filler usage efficiency and high separation performance in the simulated moving bed apparatus. The goal is to provide equipment.

The more specific purpose of the present invention to achieve the above object is to apply the chromatographic separation method industrially because conventionally, for example, the amount of processing is small even for the separation of low value-added components, or even for high value-added components. The goal is to make it practically possible to apply separation targets that could not be separated by reducing equipment costs. Alternatively, it is possible to realize this by providing a new romatoseparation method and a pseudo moving bed device that can configure a system with three unit packed beds.

Another object of the present invention is to provide an inexpensive device by simplifying control and omitting various equipment such as measuring instruments. We provide a new chromatographic separation method and a pseudo moving bed device that simplify control by dividing the operation into two steps.

Furthermore, another object of the present invention is to change the type of desorbent fluid (eluent) and to change the type of desorbent fluid (eluent), which is basically classified as a simulated moving bed type device, but which could not be realized with the conventional simulated moving bed device. The object of the present invention is to provide a new romatoseparation method and a pseudo moving bed device that can easily change the concentration.

(Means for Solving the Problems) The features of the chromatographic separation method of the present invention that achieve the above objects are as follows:
Adsorption is carried out in a chromatographic separation system in which typically two unit packed beds filled with adsorbent are connected by a fluid passage to form an endless circulation system, and communication can be cut off between the unit packed beds. Separation in which a raw material fluid containing two or more components with different affinities for the agent is supplied, the fluid is allowed to flow through the system to form a zone enriched with each component, and a fraction of the zone is extracted from the system. In the first method, communication between the unit packed beds is cut off, and a component-enriched fraction is extracted from the downstream end of the unit packed bed while supplying the raw material fluid or the desorbent fluid to the upstream end of the unit packed bed. and a second step of communicating the unit packed beds and causing the fluid to flow within an endless circulation system to form a zone enriched with each component contained in the raw material fluid.

The operations of supplying the fluid to the unit packed bed and extracting the component-enriched fraction in the first step include supplying the raw material fluid to one unit packed bed and supplying the raw material fluid to the other unit packed bed. Although it is generally preferable to perform the steps of supplying the desorbent fluid at the same time, it is also possible to perform these operations at different times.

In addition, in the second step, while the upstream side of the unit packed bed to which the desorbent particles are supplied is shut off, the desorbent fluid is supplied to one unit packed bed while the components are supplied from the other unit packed bed downstream. It is also preferable to add a third step of extracting a fraction of the zone enriched with.

The chromatographic separation method of the present invention can be carried out using two unit packed beds, but is not particularly limited to two and may be more than two.

The present invention also provides at least two unit packed beds filled with an adsorbent, a fluid passage connecting these unit packed beds to form a serial circulation path, and a fluid passage within the serial circulation path. A fluid distribution means for circulating the fluid in one direction, a cutoff valve that can be opened and closed provided in each fluid passage connecting each unit packed bed, and a raw material fluid containing two or more components having different affinities for the adsorbent. A raw material fluid supply means is provided for each unit packed bed so that it can be supplied to the upstream end of the unit packed bed, and a raw material fluid supply means is provided for each unit packed bed so that the desorbent fluid can be supplied to the upstream end of the unit packed bed. a desorbent fluid supply means; a supply fluid selection means for supplying either the raw material fluid or the desorbent fluid to the unit packed bed; and a fluid extraction means provided for each unit packed bed so that the fluid can be pulled out from the end, and the fluid selected by the supply fluid selection means is supplied to the unit packed bed by closing the cutoff valve. A step of extracting the fluid by the fluid extracting means (corresponds to the first step of the chromatographic separation method), and a step of opening the shutoff valve and circulating the fluid in the serial circulation path by the fluid circulating means (corresponding to the first step of the chromatographic separation method). The present invention is characterized by providing a simplified pseudo-fluidized bed device equipped with a switching control means for switching between a step of extracting the fluid by the fluid extracting means while supplying the fluid to the unit packed bed (corresponding to the first step of the chromatographic separation method); and a step of opening the shutoff valve and distributing the fluid within the serial circulation path by the fluid circulating means. step (corresponds to the second step of the above chromatographic separation method)
and a step of extracting a component-enriched zone fraction from the other unit packed bed while supplying the desorbent fluid to one unit packed bed by the desorbent fluid supply means (corresponding to the third step of the above chromatographic separation method). ) can also be replaced with a switching control means that switches between the two.

To explain in more detail the above chromatographic separation method and simplified simulated moving bed apparatus of the present invention, the first step involves supplying the raw material fluid or the desorbent fluid to the unit packed bed while separating both the components enriched with each other. This is a extraction step, and this operation is performed with a shutoff valve installed in the circulation channel closed to cut off circulation of the fluid in the packed bed. This process is performed to satisfy two operational requirements: supplying the raw material fluid and extracting a fraction enriched with each component. The raw material fluid is supplied from the raw material fluid supply port located near the middle of the zone enriched with components with a weak affinity for the adsorbent and the zone enriched with components with strong affinity for the adsorbent. The collected fractions are extracted from the downstream end of the unit packed bed where the zone enriched with each component is located.

In this first step, a raw material fluid is supplied to extract a fraction enriched with components having a weak affinity for the adsorbent, and in parallel with this, a desorbent fluid is supplied and a fraction enriched with components having a strong affinity for the adsorbent is extracted. Extracting the converted fraction means the following. In other words, by installing a shutoff valve between each unit packed bed and closing two of these shutoff valves at appropriate positions, one chromatography separation system that had formed a circulation loop can be separated from the raw material fluid. A chromatographic separation system from the supply section to the extraction section of the fraction enriched with components having a weak affinity for the adsorbent downstream thereof, and a chromatographic separation system from the desorbent fluid supply section to the extraction section of the fraction enriched with components having a strong affinity for the adsorbent downstream thereof. The system is divided into two chromatographic separation systems: a chromatographic separation system for both parts, and a chromatographic separation system for both parts. By being able to perform this operation, it is possible to reduce the number of unit packed beds that contribute to separation during the operation (the number of unit packed beds that are left in a state where the fluid flow has stopped, or eliminate them altogether depending on how the adsorption zones overlap). Before or after this operation, the mass balance between the feed rate of the feed fluid and the withdrawal rate of the fraction enriched in components with weak affinity for the adsorbent can be adjusted. In order to achieve this, it is also preferable to add a step of supplying a desorbent fluid and extracting a fraction enriched with components with weak affinity for the adsorbent. This can be done by closing at least one shutoff valve downstream of the outlet for both parts enriched with components with a weak affinity for the agent.

In the second step of the chromatographic separation method of the present invention, the fluid in the packed bed is circulated without supplying the fluid to the packed bed, and a zone where each component remaining in the first step is mixed or a zone where each component is mixed is formed. This is a separation process in which a dilute zone, or a zone in which the raw material fluid supplied in the first step is retained, is moved to the downstream side of the flow to form a zone enriched in each component. This is carried out until the enriched zone of each component in the layer moves one unit distance from the initial state of the first step as a unit packed bed.

In other words, the above two steps are performed by dividing the conventional pseudo-moving bed separation operation into two steps. By dividing the steps into two in this way, control is simplified and equipment costs are reduced (possibly At the same time, it uses the same principle of a moving bed as the conventional pseudo moving bed, increasing the utilization efficiency of the packing material and making it possible to obtain high separation performance that could not be achieved with batch-type chromatographic separation equipment. Furthermore, according to the present invention, it is possible to configure a system with two unit packed beds, which was not possible with conventional pseudo-moving beds, and it is possible to separate components with low added value or components with high added value. Even for the separation of targets for which it is difficult to introduce expensive equipment due to the small throughput, it is possible to provide equipment that is relatively inexpensive and easy to control, so it can be applied on an industrial scale. can be realized.

In the present invention, various types of adsorbents can be used as fillers without particular limitation, and in gas, ? ? ! It can be used as a method to separate each component in the body into two or more components enriched with each component. It is particularly suitable for separating and purifying various sugars or sugar alcohol mixtures, and for separating acids and their salts using strongly basic anion exchange resins as adsorbents.

Specifically, separation of sucrose and other useful substances from molasses, fractionation of isomerized sugar into glucose and fructose, separation of each component from a mixture containing lactose and lactulose, including sucrose and fructooligosaccharide. Separation of each component from a mixed solution, separation of each component from a mixed solution containing maltose and maltodextrin, separation of each component from a mixed solution containing sugar alcohols such as sorbitol and maltitol, mixed solution of hydrochloric acid and its salts Separation into each component from a mixture of sulfuric acid and its salts, separation into each component from a mixture of phosphoric acid and its salts, separation of two or more components such as hydrochloric acid and sulfuric acid, etc. It can be applied to the separation of acids and salts from a mixed solution of mixed acids and their salts.

(Example) The present invention will be described below based on embodiments shown in the drawings.

FIG. 1 is a diagram showing an outline of the configuration of a simplified pseudo moving bed device according to the present invention, and in this figure, 1 and 2 are unit packed beds, and 5 is a system in which these unit packed beds are circulated in an endless series. A fluid passage connected to the system, 3 a circulation pump for circulating fluid within this serial circulation system, 41 and 42 a shutoff valve that can communicate and shut off the fluid passage between the unit packed beds 1.2. It is.

6f is a pipe for supplying the raw material fluid, and is provided so that the raw material fluid f can be supplied from the upstream end thereof to each of the unit packed beds 1.2 through the raw material fluid supply valves if and 2f. . 6d is a pipe for supplying desorbent fluid, and as in the case of supplying the raw material fluid above, it is supplied to each unit packed bed 1.2 from its upstream end via desorbent fluid supply valves 1d and 2d. It is provided to be able to supply a desorbent fluid d.

6a is a pipe for extracting component A, which has a weak affinity for the adsorbent, from the unit packed bed, and extracts the enriched fraction of component A from the downstream end of each of the unit packed beds 1.2 through extraction valves 1a and 2a. It is provided so that it can be extracted. 6b is a pipe for extracting component B, which has a strong affinity for the adsorbent, from the unit packed bed, and similarly to the above, the component B is extracted from each unit packed bed 1.2 from its downstream end via the extraction valves 1b and 2b. It is provided so that the collected fraction can be extracted.

Note that the above-mentioned cutoff valves 41, 42, supply valves 1d, If,
2d, 2f, extraction valve 1a, lb, 2a, 2
b and the circulation pump 3 are arranged to repeatedly perform the first and second steps described below with reference to FIG. 2 in accordance with a predetermined sequence program determined in advance by a control device (not shown). There is.

The diagram of the first step (start) in FIG. 2 shows that a zone enriched with the A component is formed in the first half (downstream side) of the packed bed 2, and the second half (
A mixed zone of component A and component B is formed in the upstream part), a zone enriched with component B is formed in the first half of the packed bed 1, and a zone enriched with component B is formed in the second half. It shows a state where there is a zone filled with fluid, and from this state the first
The process begins.

In this diagram of the first step (beginning), the shutoff valve 41 in FIG.
．． 42 is closed, and in this state, a desorbent fluid is supplied to the packed bed 1 from the upstream end by opening the supply valve 1d, and a fraction enriched in the B component is extracted from the downstream end and then passed through the valve 1.
b. Further, the raw material fluid F is supplied to the packed bed 2 from the upstream end by opening the supply valve 2d, and a fraction enriched in component A is extracted from the downstream end via the extraction valve 2b. Note that the operations of supplying fluid to the packed beds 12 and depressurizing them can be performed at different times for the packed beds 1 and 2, if necessary.

The operation of this first step is such that the zone of each component in the packed bed is
This process is continued until the state of the first step (end) in the figure is reached.

As described below, in the first step, a raw material fluid is supplied to the simplified simulated moving bed apparatus shown in FIG. 1, which forms a zone enriched with components A and B, and This is a process of extracting a fraction enriched with H components, and the amount of fluid supplied, the amount of fluid extracted, and the operation time from the start to the end of the process are time-controlled based on experimentally confirmed data. Alternatively, an appropriate sensor can be provided at the extraction port and control can be performed based on the sensor information, and experience with known pseudo moving bed devices can also be utilized.

When the state shown in the first step (end) in FIG. 2 is reached, the supply valves 1d, 2f and the extraction valves 1b, 2
The closing of a and the opening of the shutoff valves 41 and 42 are performed by a command from a control circuit (not shown), and the circulation pump 3 is operated at the same time. As a result, in the simplified pseudo moving bed device shown in FIG. 1, fluid circulates within the circulation system without any fluid entering or exiting from the outside.

The circulation of this fluid is such that, for example, among the components in the packed bed 2 shown in the diagram of the first step (end) in FIG. This is continued until the downstream end position of No. 1 is reached. At this time, component B, which has a strong affinity for the adsorbent, moves more slowly than component A, so it will be distributed from the middle of packed bed 1 to the middle of packed bed 2, especially In the packed layer 2, a zone is formed in which only component B is enriched. The state where this circulation is completed is shown in the second step (end of circulation) in FIG.

The state of distribution of each component in the packed bed in the diagram of the second step (end of circulation) in FIG. 2 is different from the diagram of the first step (beginning) in FIG. The filling layer 2 is the same as the filling layer 1. Therefore, the raw material fluid F is supplied to the packed bed and the desorbent fluid is supplied to the packed bed L.

The feed for 2 is reversed from the first step (beginning) in FIG. 2, and the enriched components of the fraction to be extracted are similarly
Components A and B are extracted by performing the same operation as in the first step except that the first step (beginning) in the figure is reversed.
The inside of the packed bed is in the state of the first step (end), which is the fourth step from the top in FIG.

Thereafter, by performing the same operation as in the second step, the inside of the packed bed becomes the state of the second step (end of circulation), which is the fifth step from the top in FIG.

As described above, the first part of the operation of the simplified pseudo moving bed apparatus of this embodiment is explained.
After the cycle is completed, by repeating this cycle, components A and H contained in the raw material fluid can be easily separated.

As is clear from the description of the embodiments above, the simplified simulated moving bed device of the present invention utilizes a simulated moving bed in principle, but the raw material fluid is supplied to each unit packed bed. The idea of a pseudo-moving bed method is adopted in that the operations such as desorbing fluid and supplying desorbent fluid are switched (the first step), and the fluid is circulated within the circulation system without entering or exiting the fluid from outside the system. It can also be said that the idea of a batch method was adopted in that a band enriched with each component was formed (second step), and batch chromatography and pseudo-moving bed chromatography, which had previously been considered almost impossible, were adopted. It has the great significance of providing an eclectic separation technology for the first time.

The apparatus of the present invention is typically realized by the embodiment described in FIGS. 1 and 2 above, but it goes without saying that it is not limited to this embodiment. Furthermore, even when using a device that forms the same circulation system as described above, it is possible to implement an excellent chromatographic separation method that is more suited to the actual situation by changing the operating method specified by the control circuit. It is.

For example, the apparatus and chromatographic separation method described in FIG. 1 and FIG. However, in the relationship between raw materials and components that are required to be separated industrially, the amount of enriched fractions extracted from each component due to dilution with the desorbent fluid is greater than the amount of raw material fluid supplied. There are few cases where this should be considered.

FIG. 3 is for explaining a chromatographic separation method proposed to concretely solve such a problem to be considered. The characteristics of the chromatographic separation method explained in Figure 3 are:
Regarding the first and second steps, the timing of stopping the operation is slightly different from that in Figure 2, but the operating principle itself is the same as that explained in the flowchart in Figure 2. The difference is that three steps are added.

That is, this third step is a step that is performed following the second step, and is a step in which component A is extracted from another unit packed bed while supplying desorbent fluid to one unit packed bed. The problem that the amount of the fraction enriched in each component drawn out is larger than the amount of the raw material fluid supplied because it is diluted with the fluid can be solved by the operation of the third step.

Examples of the present invention will be described in more detail below, but the present invention is not limited to the following embodiments unless it departs from the gist thereof.

Example 1 Using the apparatus shown in FIG. 1, following the operations explained in FIG.
Separation was carried out using a mixed aqueous solution of sulfuric acid and its salt, sodium sulfate, having the composition shown in Table 1 as a raw material fluid, and demineralized water as a desorbent fluid.

A strongly basic anion exchange resin (Amberlite HN-1408) was used as the adsorbent packed in the unit packed bed.

The inner diameter of each of the two unit packed beds is 1000 mm, the packed bed height is 1000 mm, and both are the same. A total of 15.712 adsorbents are packed, and the operating temperature is maintained at 20 ° C.
In the configuration of this example, in which the separation operation was repeatedly performed with the time schedule shown in Table 2 and the flow rate controlled to the flow rate shown in Table 3, the order of strength of affinity with the adsorbent was as follows:
The order is sulfuric acid > sodium sulfate, and the extraction section (la,
A fluid rich in sodium sulfate is taken out from 2a), and a fluid rich in sulfuric acid is taken out from the extraction part (lb, 2b).

After repeating the operations in Table 2 for 4 cycles, the composition of each fraction in the 5th cycle was analyzed and the results are shown in Table 4.
It was shown to. From the results in Table 4, it was confirmed that the mixed solution of sulfuric acid and its salt, sodium sulfate, was efficiently separated into its respective components.

Table 1 Table (Effects of the Invention) According to the chromatographic separation method of the present invention, the separation operation performed in the conventional pseudo-moving bed is replaced by a step of transferring fluid to and from the outside of the device, and a step of transferring fluid in and out of the device. By dividing the process into steps in which fluid is circulated within the device without performing the process, it is possible to provide inexpensive equipment that can be easily controlled and operated.

In addition, the system can be configured using only two unit packed beds, which could not be achieved with conventional pseudo-moving bed equipment, and from this point of view, it is possible to provide inexpensive equipment and load handling, for example, with low added value. It has the effect of being able to provide inexpensive membrane attachment for separation of components, or for separation targets for which it is industrially difficult to introduce expensive equipment due to the small amount of processing even if the product has high added value. be.

Furthermore, the fluid inlet and the outlet of each quarter are moved as the zone enriched with each component and the zone where each component is mixed in the force separation process move downstream of the flow. Since the operation is carried out using the so-called pseudo moving bed method, the entire filler layer can be effectively involved in the separation at all times.
Compared to the batch method, it is possible to obtain much higher utilization efficiency 9 separation performance when the amount of filler is the same.

Furthermore, the same operations as the batch method (such as changing the concentration of the desorbent fluid or changing the type of desorbent fluid as in the so-called step method or gradient method) are different from the conventional pseudo moving bed method. It also has the effect of being easier to carry out compared to the method shown in Fig. 3, in which the concentration and type of the desorbent fluid supplied in the first step and the desorbent fluid supplied in the third step are changed. This can be done extremely easily.

[Brief explanation of drawings]

Figure 1 is a diagram showing an overview of the configuration of the simplified pseudo moving bed apparatus of the present invention - an example thereof, and Figures 2 and 3 show chromatographic separation that can be performed using the apparatus shown in Figure 1. 2 is a flowchart illustrating an example of the operation of FIG. 1.2: Unit packed bed la, 2a, lb, 2b: Extraction valve ld, 2d:
Raw material fluid supply valves if, 2f: Desorbent fluid supply valve 3: Circulation pump 5: Fluid passage 6a: A component extraction piping 6b: B component extraction piping 6d: Desorbent fluid supply piping 6f: Raw material fluid supply piping 41, 42: Shutoff valve (4 others) ℃ ■ 2゜4゜Indication of the case 1990 Patent Application No. 267069 Name of the invention Chromatographic separation method and simplified pseudo-moving bed device Corrected case Relationship to the case Patent applicant name ( 440) Organo Co., Ltd.

Claims (1)

[Claims] 1. A chromatographic separation system in which at least two unit packed beds filled with adsorbent are connected by a fluid passage to form an endless circulation system, and communication can be cut off between the unit packed beds. A raw material fluid containing two or more components with different affinities for the adsorbent is supplied to the system, and the fluid is allowed to flow through the system to form a zone enriched with each component, and a fraction of the zone is removed from the system. In the separation method, the communication between the unit packed beds is cut off, and the component-enriched fraction is extracted from the downstream end of the unit packed bed while supplying the raw material fluid or the desorbent fluid to the upstream end of the unit packed bed. The method is characterized in that the first step of extracting the raw material fluid and the second step of communicating the unit packed beds and circulating the fluid in an endless circulation system to form a zone enriched with each component contained in the raw material fluid are repeated. Chromatographic separation method. 2. The first step of claim 1 and the unit packed bed are communicated,
In addition to the second step of circulating the fluid in an endless circulation system to form a zone enriched with each component contained in the raw material fluid,
A chromatographic separation characterized in that a third step is performed in which the unit packed beds are communicated with each other and a desorbent fluid is supplied to one unit packed bed while a component-enriched zone fraction is extracted from another unit packed bed. Law. 3. The chromatographic separation method according to claim 1 or 2, characterized in that the number of unit packed beds is two or three. 4. The chromatographic separation method according to claim 1, wherein the raw material fluid is a mixed aqueous solution of an acid and its salt, and the adsorbent is a strongly basic anion exchange resin. 5. At least two or more unit packed beds filled with adsorbent, a fluid passage connecting these unit packed beds to form a serial circulation path, and a fluid flowing in one direction within the serial circulation path. a fluid circulation means that allows the fluid to flow; and a shutoff valve that can be opened and closed, and that is provided in each of the fluid passages that connect the unit packed layers.
A raw material fluid supply means provided for each unit packed bed so that a raw material fluid containing two or more components having different affinities for the adsorbent can be supplied to the upstream end of the unit packed bed, and a desorbent fluid supplied to the unit packed bed. a desorbent fluid supply means provided for each unit packed bed so as to be able to supply the fluid to the upstream end of the unit packed bed; a supply fluid selection means for supplying either the raw material fluid or the desorbent fluid to the unit packed bed; fluid extraction means provided for each unit packed bed so that the fraction of the zone enriched in components can be extracted from the downstream end of the unit packed bed; a step of extracting the fluid by the fluid extracting means while supplying the fluid selected by the supply fluid selecting means to the unit packed bed; and a step of opening the shutoff valve and causing the fluid to flow within the serial circulation path by the fluid circulating means. 1. A simplified pseudo-moving bed device characterized in that it is provided with a switching control means for switching. 6. In place of the switching control means of claim 5, a step of closing the cutoff valve and extracting the fluid by the fluid extraction means while supplying the fluid selected by the supply fluid selection means to the unit packed bed; A step of opening the circuit and circulating the fluid in the serial circulation path by the fluid distribution means, and enriching the component from the other unit packed bed while supplying the desorbent fluid to one unit packed bed by the desorbent fluid supply means. 1. A simplified pseudo-moving bed device, characterized in that it is provided with a switching control means for switching between a step of extracting a fraction of a zone and a step of extracting a fraction of a zone. 7. The simplified pseudo moving bed device according to claim 5 or 6, characterized in that there are two unit packed beds.