JP2001083131A - Method and device for separating a plurality of components contained in liquid - Google Patents

Abstract

PROBLEM TO BE SOLVED: To reduce the influence of a pressure loss without deteriorating the performance of chromatographic resolution when a plurality of components contained in a raw material liquid is resolved by the chormatographic resolution. SOLUTION: At the time of performing chromatographic resolution, one unit packed bed 6 packed with an adsorbent having a low moisture holding ability and a plurality of unit packed beds 1-5 and 7-10 packed with an adsorbent having a high moisture holding ability and a small grain size are connected to each other so as to form a closed loop through which a raw material liquid flows endlessly. Then a first step of extracting a prescribed component from the liquid while the liquid is supplied to the packed bed 6 and a second step of extracting the component to the outside of the system while a supernatant liquor is supplied to either one of the beds 1-10 are performed and a mass balance is maintained between the raw material liquid and supernatant liquor.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method and an apparatus for separating a plurality of components contained in a fluid which are typically applied to a simulated moving bed system, for example, a chromatographic method for producing maltose used in a starch sugar refining process. The present invention relates to a method and an apparatus suitably used for a separation operation.

[0002]

2. Description of the Related Art A method of separating a plurality of components contained in a fluid by a chromatographic technique using a solid adsorbent and utilizing the difference in the adsorption characteristics of the adsorbent (hereinafter referred to as "chromatographic separation method"). Has been conventionally used industrially. In the chromatographic separation method, basically, a raw material liquid containing two or more components to be separated is supplied to an adsorbent packed bed filled with an adsorbent, and the raw material liquid is supplied to a desorbing agent such as water (eluent). ), The components having low adsorptivity (affinity) flow relatively quickly due to the difference in the adsorptivity of each component to the adsorbent, while the components having strong adsorptivity relatively It is based on the principle that the components of each component are separated by flowing down slowly.

However, industrially, it is desired that the concentration and purity of the component to be separated and recovered be as high as possible. In many cases, a batch-type chromatographic separation method for separating and recovering components is not sufficient, and various proposals have been made for devising the above-described basic chromatographic separation operation.

[0004] For example, a number of unit packed beds are connected in series circulation so as to form a closed loop, and a supply position of a raw material liquid and a desorbing liquid (eluent) and a withdrawal position of a fraction of each component are determined. A so-called simulated moving bed system in which separation is carried out continuously while switching to the downstream side of the liquid circulation flow with respect to a unit packed bed (JP-A-62-91205, JP-A-2-124895, etc.) A method in which a step of extracting one component and a step of extracting the remaining components in order to separate three or more components are performed stepwise (Japanese Patent Publication No. 24724/1995).
Japanese Patent Application Laid-Open Publication No. 2000-157, etc.), various methods belonging to an improved method of simulated moving bed type chromatographic separation in which the supply position of a raw material liquid and a desorbing liquid (eluent) and the extraction position of a fraction of each component are switched. ing.

In addition, a plurality of unit adsorbent packed beds are connected endlessly so as to form a closed loop, and the liquid is supplied to the endless system without changing the supply position of each liquid and the extraction position of each component. (Japanese Patent Application Laid-Open No. 55-61903, etc.) has also been proposed in which each component in the supplied raw material liquid is separated while flowing the solution.

[0006] In these methods, the batch method in which the raw material liquid and the desorbed liquid are supplied to one end of a packed bed and the liquid is discharged from multiple ends is in principle common as a chromatographic separation method.
The difference is that the liquid flows through an endless path, and is superior to the batch method in that the recovered components can be separated into industrially important high productivity, high concentration and high purity.

[0007]

By the way, in the chromatographic separation method, in order to increase the productivity, it is desired to use the liquid in a condition where the liquid passing speed is set as high as possible. It is common to have a proportional relationship to the amount of total adsorbent volume. However, as described in JP-A-4-363102,
For example, when the raw material liquid is a sugar liquid or the like, when the raw material liquid is moved at a high speed due to the property that the viscosity and / or osmotic pressure of the high-concentration sugar raw material liquid supplied to the endless circulation system is high,
An excessive pressure loss may occur in the packed bed, and the device may not be operated properly. In order to solve such problems, reduce the circulation amount and supply flow rate,
A method of slowly expanding the supplied raw material liquid. Methods of supplying the raw material liquid at a low concentration have been considered.In these methods, the pressure loss of the raw material liquid supply packed bed can be kept low, but on the other hand, there is a problem that the processing time is longer in the former. However, the latter has a problem that the processing amount is reduced. Therefore, Japanese Patent Application Laid-Open No. Hei 4-363102
In the publication, the concentration of the raw material liquid component in the system is maximum when the raw material liquid is supplied (therefore, the pressure loss is also maximum), and it is noted that the concentration decreases as the operation of extracting the separated component is performed with time. To a low state over time, and proposes a method to increase the circulation flow rate in the system and the supply flow rate of the desorbed liquid over time, thereby avoiding problems such as equipment stoppage due to pressure loss and processing. The problem that the amount is small and the problem that the processing time becomes long are improved.

[0008] However, the proposed method still has room for improvement. That is, although the above method is within the limited range, since there is a portion that reduces the speed of passing the liquid in the system, it is possible to avoid prolonging the processing time to a certain extent or reducing the processing amount. Because there is no.

[0009] Apart from the above, it is conceivable to set the temperature of the solution in the system to be high in order to reduce the viscosity. Since the temperature is increased, it is difficult to employ a temperature rise more than that because thermal decomposition of the separated component is considered.

According to the present invention, in the separation of a plurality of components by the above-described chromatographic separation method, the state of the liquid passed during the supply of the raw material liquid into the system and the withdrawal of each component from the system is removed. A plurality of liquids contained in a liquid in which the influence of (component concentration, etc.) changing over time due to the separation of each component or extraction to the outside of the system, particularly the effect of pressure loss, can be reduced as much as possible without impairing the separation performance. The purpose of the present invention is to provide a novel method and apparatus for separating components.

[0011]

The present inventors have conducted various studies to achieve the above object and found that pressure loss is affected by the swelling ratio of the adsorbent. In addition, it has been found that the separation performance of the adsorbent is also affected by the magnitude of the swelling rate, and the influence of the pressure loss of the former can be suppressed when the swelling rate of the adsorbent is small,
It has been found that when the swelling ratio is small, the diffusion of the desorbed liquid in the adsorbent decreases, so that the separation performance of the latter decreases.

Therefore, an adsorbent having a small swelling ratio is used as the adsorbent of the unit packed bed at the feedstock liquid supply position where the influence of pressure loss is large, and the separation performance of the entire apparatus is applied to the unit packed bed to which no other feedstock is supplied. In order to prevent the decrease of the water content, the present invention described in each claim of the above-mentioned claims, in which an adsorbent having a large swelling ratio and a good separation performance is used.

A feature of the method for separating a plurality of components contained in a liquid according to claim 1 of the present invention is that a unit packed bed of an adsorbent through which a raw material liquid containing two or more components having different adsorbing properties to the adsorbent flows. A plurality of unit packed beds packed with at least one unit packed bed filled with a relatively small adsorbent and a relatively large adsorbent filled with a solvent,
The liquid is connected so as to form a closed loop in which the liquid flows endlessly over these unit packed beds, and the unit liquid packed with the adsorbent having a relatively small solvent holding capacity is supplied to the raw material liquid with respect to the closed loop system. And the operation of supplying the desorbed liquid to any of the unit packed beds, and the operation of flowing the raw material liquid and the desorbed liquid in one direction through the endless closed loop system using a pump. The enrichment by separating components having different absorptivity contained in the raw material liquid supplied into the closed loop in the direction of the flow of the liquid in the closed loop system, and separating the enriched components into fractions. Extracting from the closed loop while maintaining the mass balance with the supply of the raw material liquid and / or the desorbed liquid from the unit packed bed in which the enriched fraction of each component is present. I do.

In the above, the term "adsorbent" refers to an agent having a chromatographic separation function for components contained in a raw material liquid, such as a gel type strongly acidic cation exchange resin and a gel type strongly basic anion exchange resin. A synthetic adsorbent having no ion exchange ability, such as an ion exchange resin and a styrene-divinylbenzene copolymer, can be exemplified. The adsorbent may be referred to as a separating agent, a sorbent, a desorbing agent, a filler or the like used in the chromatographic separation method, but is not distinguished from the adsorbent in the present invention.

[0015] "Adsorption" of a plurality of components contained in the raw material liquid to the adsorbent (this adsorbability is sometimes referred to as "affinity" of each component to the adsorbent).
In other words, the difference is that the movement speed when each component moves in contact with the adsorbent is different depending on the physical and chemical characteristics, and this means that when the raw material liquid moves in the closed loop, The components having different moving speeds with respect to the adsorbent contained in the raw material liquid are separated in the moving (flow) direction.

The "unit packed bed" basically refers to one unit packed with the same adsorbent. In an industrial apparatus, a fixed pressure vessel such as a packed tower is used. Adsorbent packed in a column (tank, tower) composed of

The present invention has a characteristic configuration in which two types of adsorbents having different properties with respect to the solvent holding capacity are used. In this specification, the term "solvent holding capacity" means the following. That is, water used for the desorbing solution, an organic solvent such as an aqueous solution of alcohols (for example, an aqueous methanol solution, an aqueous ethanol solution, an aqueous 2-propanol solution), or an aqueous acetone solution is contained in the pores (micropores and macropores) of the porous resin. Is the amount (at saturation equilibrium) retained in a solvent, which has a correlation with the degree of resin crosslinking, and the degree of swelling of an adsorbent with a certain solvent holding capacity is proportional to this solvent holding capacity The swelling rate of the adsorbent having a large solvent holding capacity is large and the separation performance is excellent. On the other hand, the swelling ratio of an adsorbent with a small solvent holding capacity is small, so the separation performance is low, but the effect of the osmotic pressure caused by the change in the concentration of the liquid surrounding the adsorbent is small, and it is harder than the adsorbent with a large swelling ratio Therefore, the rise in liquid flow resistance is small. In addition,
When the adsorbent is an ion exchange resin, the water holding capacity when water is used as a solvent (solvent holding capacity) differs depending on the ionic form. It refers to possession ability. Specifically, the solvent is water, and the strongly acidic cation exchange resin is sodium ion form, the weakly acidic cation exchange resin is hydrogen ion form, the strong basic anion exchange resin is chloride ion form, and the weak basic anion The exchange resin has a free base form (hydroxide ion form) as a reference ion form.

Regarding the solvent holding capacity, the adsorbent of the unit packed bed to which the raw material liquid is supplied in the present invention and the solvent holding capacity of the adsorbents of the other unit packed beds are “relatively small”.
Alternatively, “relatively large” refers to a relative relationship between them, such as the number of unit packed beds that supply a raw material liquid among a plurality of unit packed beds, and thus the ratio of the amounts of these adsorbents. Therefore, the magnitude relationship (ratio) between the solvent holding capacities of the adsorbents having different solvent holding capacities is not necessarily determined uniformly, but is particularly limited as long as the separation performance of the entire apparatus is within a range that can be satisfied. It is possible to design empirically and theoretically, but in general,
It is often better to be 1.5, preferably 1.1-1.3.

In the case where a strongly acidic cation exchange resin is used as the adsorbent and the solvent is water, a relatively small adsorbent of the reference ion type (sodium ion type) has a solvent holding capacity of 45 to 45. 50%, preferably 47-50%
In many cases, the relatively large adsorbent has a solvent holding capacity of 51 to 60%, preferably 53 to 60%.
It is often better to be 57%.

If the former (solvent holding capacity is relatively small) adsorbent has a solvent holding capacity of less than 45%, the diffusion within the adsorbent is reduced, so that the selectivity to the component to be separated is reduced, and the separation performance is reduced. However, if the ratio exceeds 50%, the swelling is large and the rise in liquid flow resistance is large. Also, if the latter (solvent holding capacity is relatively large) adsorbent has a solvent holding capacity of less than 51%, diffusion within the adsorbent is insufficient, resulting in insufficient separation performance. Although the performance is excellent, the rise of the liquid flow resistance becomes remarkable and a large pressure loss is caused, so that the above range is set.

The ratio of the adsorbent having a relatively small solvent holding capacity to the total amount of the adsorbent in the entire apparatus may be substantially determined according to the operation method of the chromatographic separation method used. Industrially, from the viewpoint of ease of operation control, it is common to pack adsorbent into packed columns (columns) of the same capacity to form individual unit packed beds. More than a fraction of the packed bed (in this case, only one unit packed bed is filled with adsorbent with low solvent holding capacity) and 50% (in this case, half of the endlessly connected unit packed beds are solvent holding capacity Filled with a small adsorbent)
It is often better to:

It is necessary that the unit packed bed for supplying the raw material liquid is always filled with an adsorbent having a relatively small solvent holding capacity. However, it is not always necessary to use a unit packed bed that always supplies a raw material liquid. That is, it is preferable that the unit packed bed in which the pressure loss becomes a problem is filled with an adsorbent having a smaller solvent holding capacity than that of an adsorbent having a relatively large solvent holding capacity. In a chromatographic separation method in which the raw material liquid is supplied to only one of the unit packed beds, a unit packed bed for supplying the raw material liquid and one or two unit packed beds following the unit packed bed (this includes the raw material liquid) (It is not directly supplied.) It is preferable that the solvent holding capacity is relatively small.

The method of the present invention is disclosed in JP-A-62-9120.
No. 5, publication No. 5, etc., which can be applied by modifying the above method based on a general simulated moving bed type chromatographic separation method, and a step of extracting one component in order to separate three or more components. And a method of performing a step of extracting the remaining components in a stepwise manner (Japanese Patent Publication No. 24724/1995) and the like, and can also be applied to a simulated moving bed type chromatographic separation method in a modified mode, and further uses a closed loop system. If it is a chromatographic separation method, it can be applied to a method other than the simulated moving bed method. As a chromatographic separation method other than the simulated moving bed method, for example, a method described in JP-A-55-61903 can be exemplified. To give a more specific example,
The four adsorbent columns (unit packed beds) are connected endlessly so as to form a closed loop system, supply of desorbed liquid from the top of the first column, and feed from the top of the third column It is possible to supply a liquid, withdraw a fraction liquid containing one separated component from the end of the first column, and withdraw a fraction liquid containing another separated component from the end of the third column. And a first step of supplying a raw material liquid from the top of the third column and extracting a component having low adsorptivity from the end of the third column. A second step of endlessly circulating the liquid in the direction, a third step of supplying a desorbed liquid from the top of the first column, and extracting a component having a high adsorptivity from the column end of the first column,
In the method in which the four steps of the fourth step of supplying from the top of the tower and extracting the weakly adsorbable component from the end of the third tower are repeated in this order, the adsorbent to be charged into the third tower is The above invention can be carried out by using an adsorbent having a relatively smaller solvent holding capacity than another adsorbent to be charged in another column.

The supply of the desorbed liquid is carried out not only on a unit packed bed filled with an adsorbent having a relatively large solvent holding capacity but also on a unit packed bed filled with an adsorbent having a relatively small solvent holding capacity. Naturally, the desorbed liquid can be supplied to another unit packed bed simultaneously with the supply of the raw material liquid.

According to the present invention, it is possible to prevent a problem associated with the occurrence of pressure loss at the time of supplying the raw material liquid without causing a large decrease in separation performance.

According to a second aspect of the present invention, in the above invention, an adsorbent having a relatively large solvent holding capacity is filled downstream of the liquid flow of a unit packed bed filled with an adsorbent having a relatively small solvent holding capacity. One or more unit packed beds are connected.

According to the present invention, for example, in a simulated moving bed apparatus in which the total number of unit packed beds is eight, the unit packed bed filled with an adsorbent having a relatively small solvent holding capacity and the solvent holding capacity are relatively small. The unit liquid beds with large adsorbents are connected alternately every other unit, and the raw material liquid is supplied to the unit packed beds filled with adsorbents with relatively low solvent holding capacity among the endlessly connected unit packed beds. However, do not supply to a unit packed bed filled with an adsorbent having a relatively large solvent holding capacity. In addition to this, supply positions of raw material liquid and desorbed liquid, and extraction positions of each component outside the system Can be performed by performing a general pseudo-moving-bed type operation of sequentially switching over time to the downstream side of the circulation flow.

According to a third aspect of the present invention, in the above-mentioned invention, the closed loop system includes one of a unit packed bed filled with an adsorbent having a relatively small solvent holding capacity and an adsorbent having a relatively large solvent holding capacity. Endlessly connected to a plurality of unit packed beds filled with, and while supplying the raw material liquid to the unit packed bed filled with the adsorbent having a relatively small solvent holding capacity, the fraction of enriched components A step of performing an operation of extracting the liquid out of the closed loop, and stopping the supply of the raw material liquid to the unit packed bed, and supplying the desorbed liquid to any of the other unit packed beds while enriching the components. Performing the operation of extracting the fraction liquid out of the closed loop.

The present invention is preferably implemented, for example, as a method in which a step of extracting one component and a step of extracting the remaining components are performed in a stepwise manner in order to separate three or more components. That is, a closed loop circulation path is formed using a large number of unit packed beds filled with the adsorbent,
And this circulation flow path is a system that is provided so as to be able to circulate and shut off, by passing a raw material liquid containing three or more components having different adsorbents to the adsorbent through the plurality of unit packed beds, For a system that forms an adsorption zone that is sequentially divided into components that have low adsorptivity to strong adsorbent, upstream of the adsorption zone that is formed by components selected in advance among components that have low adsorbability While substantially blocking the circulation of the system at the position, a unit packed bed filled with an adsorbent having a relatively small solvent holding capacity is arranged downstream of the blocked position to supply the raw material liquid, A first step of extracting a fraction enriched with a predetermined component from among the components forming the adsorption zone upstream of the shut-off position from the system, and circulating the system without supplying a raw material liquid. Adsorption remaining in the first step A second step of separately extracting the enriched fraction of each component divided into zones while supplying a desorbing solution according to a method of a two-component simulated moving bed, and repeating each step as one cycle. Can be configured.

According to the present invention, while suppressing the effect of the pressure loss, the overall separation capacity of the adsorbent having a relatively large solvent holding capacity in a unit packed bed other than the unit packed bed for supplying the raw material liquid. , It can be kept in a high state.

In the first step, while the raw material liquid is supplied, the distribution of the adsorption zone of each component extracted in the next cycle is formed, and the adsorptivity of the components having the adsorption zone already formed is intermediate. This is a step of extracting at least one of the fractions enriched in components classified as (hereinafter referred to as "intermediate components") out of the system, whereby a large amount of intermediate components can be extruded with the raw material liquid in a short time. In addition, since the unit packed bed for supplying the raw material liquid is filled with the adsorbent having a small water holding capacity, the effect of pressure loss can be suppressed.

In the second step, the enrichment of each target component other than the intermediate component is carried out in accordance with the "simulated moving bed method" while circulating the fluid in the system without supplying the raw material liquid. The separated fractions are separately extracted from the system, and each component contained in the raw material liquid newly supplied to the system in the first step is sequentially changed from a component having a low adsorptivity to an adsorbent to a component having a strong adsorptivity. This is a step for forming a divided adsorption zone. Here, the "pseudo-migration bed method" used for extracting each component separately while supplying the desorbing liquid is a general pseudo-migration bed method except that the supply of the raw material liquid is not performed. Well-known examples, for example,
No. 91205, particularly the second line of the upper right column to the last line of the lower left column of page 2 and the method described with reference to FIG. Except that the section and the fourth section may be considered to be the same section, the operation can be performed as it is. Specifically, while circulating the liquid in the system by a pump or the like, the desorbed liquid is supplied from the upstream of the adsorption zone in which the predetermined component is distributed, and the component-enriched fraction is supplied from the downstream of the adsorption zone. Can be carried out by sequentially performing the operation of sequentially extracting the components downstream of the circulation flow in accordance with the movement of the adsorption zone for a plurality of components other than the intermediate components.

According to the present invention, the three components having different adsorptivity contained in the raw material liquid can be separated by the unit packed bed group connected to the closed loop system and having high separation ability, and the unit for supplying the raw material liquid can be separated. Since the packed bed is filled with an adsorbent having a small solvent holding capacity, the influence of pressure loss is small. Therefore, a high-concentration raw material liquid can be supplied at high speed, and high productivity can be obtained.

According to a fourth aspect of the present invention, in the third aspect of the present invention, the operation of extracting the enriched component fraction out of the closed loop while supplying the desorbing liquid to any one of the unit packed beds is performed. The step of performing is characterized by including an operation of switching the supply position of the desorbed liquid and the extraction position of the fraction liquid to the unit packed bed on the downstream side of the liquid flow every predetermined time.

According to the present invention, a fraction of the target component can always be extracted from the system from an appropriate position where its concentration and purity are enriched. As described above, the desorbed liquid can be supplied to any unit packed bed regardless of the magnitude of the solvent holding capacity.

According to a fifth aspect of the present invention, in the above invention, the closed loop system is provided with two or more unit packed beds filled with an adsorbent having a relatively small solvent holding capacity and a downstream of each of these unit packed beds. One or more unit packed beds filled with an adsorbent with a relatively large solvent holding capacity are connected endlessly, and the raw material is placed on a unit packed bed filled with an adsorbent with a relatively small solvent holding capacity. A step of extracting the fractionated liquid of the enriched component out of the closed loop while supplying the liquid, and supplying the raw material liquid to a unit packed bed filled with the adsorbent having a relatively small solvent holding capacity. Stopping and removing the enriched component fraction from the closed loop while supplying the desorbing liquid to any of the other unit packed beds. One unit filled with a small adsorbent After performing the step of supplying the raw material liquid to the packed bed, the supply and withdrawal positions of the liquid are sequentially switched over time to the unit packed bed on the downstream side of the liquid flow, and again the one solvent holding capacity is relatively small. The process is repeated until the supply of the raw material liquid to the unit packed bed filled with the agent is started as one cycle.

According to the present invention, for example, when the total number of unit packed beds is eight and the number of unit packed beds of the adsorbent having a relatively small solvent holding capacity is two, the first and fifth units are used. The unit liquid bed can be supplied twice in one cycle as a unit packed bed of the adsorbent having a relatively small solvent holding capacity.

The invention according to claim 6 is characterized in that, in each of the above-mentioned inventions, in parallel with the operation of supplying the raw material liquid to the unit packed bed filled with the adsorbent having a relatively small solvent holding capacity, the other unit packed beds are filled. An operation of supplying a desorbed liquid is performed.

According to the present invention, each component can be efficiently extracted, and the productivity can be improved.

The invention of an apparatus for separating a plurality of components contained in a liquid according to claim 8 comprises a plurality of unit packed beds filled with an adsorbent through which a raw material liquid containing two or more components having different adsorbing properties to the adsorbent is passed. Consisting of at least one unit packed bed filled with an adsorbent having a relatively small solvent holding capacity, and a plurality of unit packed beds filled with an adsorbent having a relatively large solvent holding capacity, wherein the liquid A closed-loop system connected endlessly across the packed bed, and a raw material liquid connected to supply the raw material liquid to a unit packed bed filled with an adsorbent with relatively small solvent holding capacity in this system Supply means;
A desorbing liquid supply means for selecting one of the unit packed beds and supplying a desorbing liquid, a pump means for flowing the liquid in one direction in a closed loop system, and a raw material by flowing the liquid When the components contained in the liquid are separated and enriched in the direction of the liquid flow due to the difference in adsorptivity, the fraction liquid of the component is separated from the unit packed bed in which the fraction of the enriched component is present in the closed loop. And a liquid extracting means for extracting the liquid to the outside.

In the above arrangement, the means for supplying the raw material liquid and the desorbed liquid is generally a branch pipe from each liquid supply pipe shared by each liquid to each unit packed bed provided with an opening / closing valve. Can be configured. Similarly, the liquid discharging means for each component can be constituted by connecting a liquid discharge pipe from each unit packed bed provided with an open / close valve to a common discharge pipe for each component.

According to the present invention, basically, the solvent holding capacity of the adsorbent to be filled in each unit packed bed is selected while keeping the configuration of the conventional simulated moving bed apparatus, so that The method invention can be suitably implemented.

A ninth aspect of the present invention is characterized in that, in the above-mentioned apparatus invention, the liquid discharging means has liquid discharging means for each component contained in the raw material liquid.

In the above configuration, it is natural that the components to be separated and the other components are separately provided with a liquid extracting means, but according to the present invention, the liquid extracting means is provided for each component. By providing the components, a plurality of components can be separated from each other.

According to a tenth aspect of the present invention, in the above-mentioned apparatus, the raw material liquid supply means switches the supply / stop of the raw material liquid to a unit packed bed filled with an adsorbent having a relatively small solvent holding capacity. It is characterized by having switching means.

According to the present invention, it is possible to supply / stop the raw material liquid to the unit packed bed filled with the adsorbent having a relatively small solvent holding capacity by a simple operation.

According to an eleventh aspect of the present invention, in the above apparatus, the desorbed liquid supply means has a supply position switching means for switching a supply position for the closed loop system to a unit packed bed downstream of the liquid flow. Features.

In the above configuration, the liquid supply means for supplying the desorbed liquid is not only a unit packed bed filled with an adsorbent having a relatively large solvent holding capacity but also packed with an adsorbent having a relatively small solvent holding capacity. It can also be connected to a unit packed bed. This is because the desorbed liquid basically has no problem such as pressure loss. Therefore, when the supply position of the desorbed liquid is switched, it can be switched sequentially, if necessary, including a unit packed bed filled with an adsorbent having a relatively small solvent holding capacity.

According to a twelfth aspect of the present invention, in the above-mentioned device invention, the liquid extracting means sets a position for extracting from the closed loop,
It is characterized by having extraction position switching means for switching to a unit packed bed on the downstream side of the liquid flow.

In the present invention, the liquid can be withdrawn from the unit packed bed in which each component is well enriched, and is not affected by the solvent content of the adsorbent filled in each unit packed bed. Therefore, when switching the liquid withdrawal position, it is possible to switch sequentially including the unit packed bed filled with the adsorbent having a relatively small solvent holding capacity, if necessary.

[0051]

BEST MODE FOR CARRYING OUT THE INVENTION Hereinafter, an embodiment of the present invention will be described with reference to the drawings as an example in which components in a sugar raw material liquid are separated using a strongly acidic cation exchange resin as an adsorbent and water as a solvent. However, it is obvious that the present invention is not limited to the following embodiments unless departing from the gist thereof.

Embodiment 1 FIG. 1 shows A (maltose), B (glucose),
FIG. 1 is a view schematically showing the configuration of a simulated moving bed apparatus for separating three components of C (fructose). In FIG. 1, reference numeral 6 denotes a unit packed tower (bed) filled with an adsorbent having a relatively small water holding capacity. On the other hand, 1 to 5 and 7 to 10 each represent a unit packed column packed with an adsorbent having a relatively large water holding capacity,
Adsorption (affinity) strength of the above three components is C> B
> A is filled with a strong acidic cation exchange resin.

Each of the unit packed towers 1 to 10 is connected to a closed loop system capable of endlessly circulating liquid through a pipe 20 connected in series. The end is connected to the top of the unit packing tower 1 in the first stage via a pipe 21 of a fluid passage.

Reference numeral 19 denotes a circulating pump provided in the middle of the fluid passage 21 so that the flow rate can be controlled to a set value by a control device (not shown).

Z is a shut-off valve provided between the unit packed towers 5 and 6, and its opening and closing are controlled by a control device (not shown).

A supply valve for the raw material liquid F is provided in a pipe between the shut-off valve Z provided between the unit packed towers 5 and 6 of the packed tower group and the unit packed tower 6 downstream thereof. The raw material liquid supply pipe 30 is connected to the raw material liquid supply pipe 30 via a line f.
A common desorption liquid supply pipe 31 is connected to a pipe between the shutoff valve Z and the unit packed tower 6 via a desorption liquid supply valve 6D.

On the other hand, three pipes are connected to the pipe between the shut-off valve Z and the unit packing tower 5 upstream of the shut-off valve Z for discharging the liquid out of the system. That is, the extraction valve 5A for the component (A component) having low adsorbability to the adsorbent and the component (C component) for strong adsorption, so that each enriched component can be fractionated and extracted. Through a discharge valve 5C and a discharge valve 5B for a component having an intermediate adsorptivity (component B), the components are connected to common pipes 12, 13, and 14 for fractionated liquids of the respective components.

Between the unit packed towers 1 to 5 and 7 to 10, the common desorbed liquid supply pipe 31 is connected to the desorbed liquid supply valves 1D, 2D, 3D, 4D, 5D, 7D, 8
D, 9D, and 10D are connected so as to be able to supply the desorbed liquid to each unit packed tower, and these supply valves, together with the supply valve 6D and the raw material liquid supply valve f, are controlled by a control unit (not shown). The opening and closing are controlled by the device.

Further, between the above-mentioned unit packed towers 1 to 5, 6 to
Between 10, the common liquid extraction pipe 12 is provided with each of the A component extraction valves 1A, 2A, 3A, 4A, 6A, 7A, 8A, 9
A and 10A are connected so as to be able to extract the component A fraction liquid from each unit packed column, and the common liquid extraction pipe 14 is similarly connected to the component extraction valves 1C, 2C, 3C, 4C, 6
The components C, 7C, 8C, 9C, and 10C are connected so that a C component fraction can be extracted from each unit packed column via C.
That is, these pipes for extracting liquid are unit packed towers 1 to 5
In the case of the components A and C, the withdrawal valves 1A-
5A and a common extraction pipe 12, 1C through 1C to 5C.
4 and between the unit packed towers 6-10, the extraction valves 6A-10A and 6
The extraction valves are connected to common extraction pipes 12 and 14 via C to 10C, and the opening and closing of these extraction valves are controlled by a control device (not shown).

In the apparatus configured as described above, when the target component to be separated and recovered from the raw material liquid is the above-mentioned intermediate B component having adsorptivity, the operation of separating this B component to high purity is as follows. Done in

First, in the first step, the raw material liquid F is supplied to the unit packed bed 6 through the raw material liquid supply valve f downstream of the shutoff valve Z in the closed state, and at the same time, the desorbed liquid D is supplied. By supplying the liquid via the desorbing liquid supply valve 1D, the B component fraction is extracted from the upstream of the shutoff valve Z via the extraction valve 5B. At this time, the enriched fraction of the component A can be simultaneously withdrawn from the extraction valve 8A, and if necessary, the enriched fraction of the component C can be extracted via the extraction valve 2C. You can also.

Next, in the second step, the shutoff valve Z is opened,
While the supply of the raw material liquid F is stopped and the fluid is circulated in the system, the supply of the desorbing liquid D is performed according to the method of the simulated moving bed.
The separation of the component C and the separation of the component A are performed, and the supply position of the desorbed solution and the extraction position of each fraction are sequentially adjusted in accordance with the movement of each enriched fraction. The operation is performed to transfer one tower downstream at a time.

The operation of the second step is completed after switching the supply and withdrawal positions of the liquid nine times, and the process returns to the first step. This is repeated as one cycle.

In this embodiment, the shut-off valve Z is provided at only one location in the middle of the circulation flow path. However, it may be provided at two or more locations. The unit packed tower to which the raw material liquid is supplied from the liquid supply port is filled with an adsorbent having a small water holding capacity.

Embodiment 2 FIG. 2 is a diagram showing a schematic configuration of a simulated moving bed type chromatographic separation apparatus used for carrying out the present invention.

In FIG. 2, reference numerals 1 to 10 denote unit packed towers (beds) each filled with an adsorbent. In the case of separating saccharides, for example, in this example, 1, 3, 5, 7, and The unit packed tower of No. 9 is packed with a strongly acidic cation exchange resin having a relatively small water holding capacity, and the unit packed towers of 2, 4, 6, 8, and 10 are packed with a strong acid having a relatively large water holding capacity. Packed with a cationic cation exchange resin, unit packed columns of two different adsorbents were alternately arranged. And each of these unit packed towers 1
10 to 10 are connected in series by a pipe 20 so that the liquid can be circulated sequentially.
At the end of the first unit packing tower 1
The connection through the first unit 1 constitutes a closed loop system having an endless circulation as a whole.

Reference numeral 19 denotes a circulation pump provided in the middle of the fluid passage 21 so that the liquid flows in the circulation system in one direction shown by an arrow in the figure. The flow rate of the liquid can be controlled to a set value by a control device (not shown). The pump 19 may be installed anywhere between the unit packed towers, and may be provided as many as necessary.

In the pipes 20 and 21 between the above packed tower groups, unit packed towers 1, 3, 5, 7 and 9 filled with an adsorbent having a relatively small water holding capacity have their tops ( A raw material liquid supply unit is connected to a circulation system for supplying the raw material liquid F from the start end). That is, a common raw material liquid supply pipe is connected to the pipes 20, 21 connected to the unit packed towers 1, 3, 5, 7, 9 via the raw material liquid F supply valves 1F, 3F, 5F, 7F, 9F. The feed liquid supply pipe 15 is connected to the feed liquid supply pipe 30. In addition, a common desorbing liquid supply pipe 31 is connected to the pipes 20, 21 connected to the tops of all the unit packed columns 1 to 10 via desorbing liquid supply valves 1D to 10D, respectively. The desorbed liquid supply pump 16 is connected to the desorbed liquid supply pipe 31.

Further, the pipes 20 and 2 between the packed tower groups described above are used.
1 is connected to a liquid extracting means for extracting a liquid of a fraction containing a predetermined component from the end (end portion) of each unit packed column to the outside of the circulation system. That is, each of the pipes 20 and 21 between the unit packed towers is provided with a discharge valve 1A to 10 for a component having a low adsorptivity to an adsorbent (hereinafter referred to as “A-class liquid”).
A common section A liquid withdrawal pipe 12 is connected via A. Similarly, each of the pipes 20 and 21 between the unit packed towers is provided with a component having a high adsorptivity to the adsorbent (hereinafter referred to as “C
A common C-separated liquid extraction pipe 13 is connected via extraction valves 1C to 10C of "separated liquid").

Further, the above-mentioned raw material liquid supply valves 1F, 3F,
5F, 7F, 9F, Desorption liquid supply valves 1D to 10D, A-class liquid discharge valves 1A to 10A, C-class liquid discharge valves 1C to 10
Each valve of C is operated in a pseudo moving bed type chromatographic separation operation (ie, the adsorbent is apparently moved intermittently between the liquid supply position and the liquid withdrawal position in the liquid circulation direction, and is in the opposite direction to the liquid flow). Is controlled by a valve opening / closing control device (not shown) according to a predetermined sequence program. However, as described above, the raw material liquid is supplied only to the packed towers 1, 3, 5, 7, and 9 filled with the adsorbent having a relatively small water holding capacity.

In the apparatus configured as described above, the operation of separating the components to be separated contained in the raw material liquid into the respective fractions is performed as follows.

First, in the first step, the raw material liquid supply valve 5
The raw material liquid F is supplied to the unit packed tower 5 via F,
At the same time, the desorbed liquid D is supplied via the desorbed liquid supply valve 10D. As a result, the liquid of the fraction enriched in the weakly adsorbable component (A-class liquid) and the liquid of the fraction enriched in the strongly adsorbable component (C-class liquid) are separated in the direction of circulation. , A liquid is withdrawn from the A liquid withdrawal valve 7A, and C liquid is withdrawn from the C liquid withdrawal valve 1C.

Next, in the second step, the supply of the raw material liquid F is stopped, and the supply position of the desorbing liquid D and the withdrawal position of the A-separated liquid are adjusted in accordance with the movement of each enriched fraction. An operation to switch and shift one tower at a time to the downstream side is performed. As a result, the A-class liquid proceeds downstream in the flow of the circulating flow, while
When the adsorbent apparently moves in the opposite direction to the flow of the circulating flow by switching the valve, the C-section liquid apparently moves to the upstream side of the circulating flow. Therefore, the desorbed liquid is supplied to the unit packed tower 1 via the desorbed liquid supply valve 1D, and the A-class liquid is withdrawn from the unit packed tower 8 via the A-class liquid withdrawal valve 8A. In this case, the operation of extracting the C-section liquid may be performed in parallel. In this case, the operation may be performed by extracting the liquid from the unit packed tower 2 via the C-section liquid extraction valve 2C.

The above operation is repeated up to the tenth step by repeating the same operation as the first and second operations in this order, thereby completing one cycle of the simulated moving bed type chromatographic separation operation. Of course, this operation can be performed continuously over a plurality of cycles without being completed in one cycle.

In this example, the device shown in FIG.
Although a unit packing tower is used, the present invention is not limited to this.

[0076]

Example 1 Using the apparatus shown in FIG. 1, fructose was separated from a raw material liquid (isomerized sugar) having the following composition. The unit packed towers 1 to 10 used in this apparatus had an adsorbent layer height of 1.6 m and a total adsorbent amount of 150 liters.

Raw material liquid (isomerized sugar) Maltose purity: 5% Glucose purity: 50% Fructose purity: 45% Solids concentration: 60% The adsorbent is used for the column having a symbol 6 for chromatographic separation with a water holding capacity of 45%. The column was filled with a strongly acidic cation exchange resin (prototype resin A), and the other column was filled with a water holding capacity of 55% (prototype resin B). The ionic form was a Ca form.

The test was performed under the following conditions according to the operation method of the first embodiment. The ratio of the water holding capacity of the adsorbent (prototype resin B) / (prototype resin A) was 1.22.

Operating conditions Operating temperature: 60 ° C. First step (raw material supply step) Raw material liquid supply amount: 11.40 liters Processing time: 24.30 minutes Desorption liquid (water) supply amount: 13.30 liters Amount of the fraction extracted from the weak component (maltose): 7.60 liter Amount extracted from the fraction of the intermediate component (glucose) having the adsorptivity: 17.10 liter Second step Desorption liquid (water) supply: 5.70 liters Process time: 16.20 minutes Discharge amount of fraction of weakly adsorbable component (maltose): 2.53 liter Discharge amount of fraction of strongly adsorbable component (fructose): 3.17 Liter Fastest circulation flow rate: 39.85 liters / hr The second step is performed up to the tenth step while sequentially switching the supply position of the desorbed liquid and the extraction position of each component to the downstream side of the circulation, and returns to the first step. One cycle was performed.

The average column pressure in the above operation was as follows.

At the time of supply of undiluted solution: 3.5 kg / cm ^{2 After} the second step: 2.3 kg / cm ² The purity and recovery rate of the recovered fructose were as follows.

Recovered fructose purity: 95%, fructose recovery rate: 90
% Comparative Example 1 The same apparatus as in Example 1 was used, and the prototype resin B was packed as an adsorbent in all unit packed towers 1 to 10 and operated in the same manner as in Example 1. In addition, the same flow rate as in Example 1 (first flow rate)
When the liquid was passed at all flow rates including the feed rate of the undiluted solution in the process), the pressure loss became too large. Therefore, the apparatus was operated at a flow rate of 90% of Example 1 to protect the apparatus. The average column pressure during operation, the purity of the recovered fructose, and the recovery were as follows.

[0083] Mean tower pressure solution feed time: 4.0 kg / cm ² second step thereafter: 3.0 kg / cm ² recovery fructose purity: 95%, fructose recovery: 90% Example 1 and Comparative Example 1 As can be seen from the comparison of the test results, the adsorbent packed in the unit packed tower for supplying the raw material liquid (only the unit packed tower 6 in the example of FIG. 1) having a small water retention capacity is used, so that the separation performance ( While maintaining the same level of purity and recovery as in Comparative Example 1, the pressure loss due to the passage can be suppressed, and the pressure loss can be reduced by about 1 compared to Comparative Example 1.
It was confirmed that the liquid could be flowed at a relatively high flow rate.
Therefore, the effect that the apparatus can be miniaturized with the same processing amount is exhibited.

[0084]

According to the present invention, in a simulated moving bed type chromatographic separation method for separating a component to be separated from a raw material liquid containing two or more components into two or more fractions, adsorption having different solvent holding capacities is performed. By using the agent, there is an effect that the supply amount of the raw material liquid can be increased, and the purity and the recovery rate can be improved without impairing the separation performance as a whole.

According to the chromatographic separation method of the present invention,
The same productivity has the effect of reducing the amount of adsorbent, reducing the amount of desorbent used, shortening the processing time, and improving the purity and recovery rate of the component to be separated. There is.

Further, through these, there is an effect that the size of the chromatographic separation device can be reduced.

[Brief description of the drawings]

FIG. 1 is a diagram showing a schematic configuration of a first embodiment of a simulated moving bed type chromatographic separation apparatus in which three components contained in a raw material liquid are separated by chromatography and separated and recovered.

FIG. 2 is a diagram illustrating a schematic configuration of a second embodiment of a pseudo moving bed type chromatographic separation apparatus in which two components contained in a raw material liquid are separated by chromatography and separated and recovered.

[Explanation of symbols]

1 to 10: Unit packed tower 1A to 10A: Extraction valve for A segment liquid 5B: Extraction valve for B segment liquid 1C to 10C: Extraction valve for C segment liquid 1D to 10D: Desorption liquid supply valves 1F, 3F, 5F, 7F, 9F, f: raw material liquid supply valve A: A-class liquid (liquid with high content of component flowing out first) B: B-class liquid (liquid with high content of component flowing out in the middle) C: C Classified liquid (liquid with a high content of the last component flowing out) D: Desorbed liquid F: Raw material liquid Z: Shut-off valve 12: Pipe for extracting A-class liquid 13: Pipe for extracting B-class liquid 14: C-class liquid Extraction pipe 15: Raw material liquid supply pump 16: Desorption liquid supply pump 19: Circulation pump 20, 21: Piping 30: Raw material liquid supply pipe 31: Desorption liquid supply

[Procedure amendment]

[Submission date] July 25, 2000 (2007.2
5)

[Procedure amendment 1]

[Document name to be amended] Statement

[Correction target item name] Claims

[Correction method] Change

[Correction contents]

[Claims]

[Procedure amendment 2]

[Document name to be amended] Statement

[Correction target item name] 0022

[Correction method] Change

[Correction contents]

It is necessary that the unit packed bed for supplying the raw material liquid is always filled with an adsorbent having a relatively small solvent holding capacity. However, it is not always necessary to use a unit packed bed that always supplies a raw material liquid. That is, it is preferable that the unit packed bed in which the pressure loss becomes a problem is filled with an adsorbent having a smaller solvent holding capacity than that of an adsorbent having a relatively large solvent holding capacity. In a chromatographic separation method in which the raw material liquid is supplied to only one of the unit packed beds, a unit packed bed for supplying the raw material liquid and one or two unit packed beds following the unit packed bed (this includes the raw material liquid) It is preferable that an adsorbent having a relatively low solvent holding capacity is filled in the adsorbent ( not directly supplied).

[Procedure amendment 3]

[Document name to be amended] Statement

[Correction target item name] 0050

[Correction method] Change

[Correction contents]

[0050] In the present invention, extraction of the liquid can be carried out from the unit packed bed in a state where each component is favorably the wealth Yutakaka not affected by the solvent holdings ability of the adsorbent filled in the respective unit packed beds . Therefore, when switching the liquid withdrawal position, it is possible to switch sequentially including the unit packed bed filled with the adsorbent having a relatively small solvent holding capacity, if necessary.

[Procedure amendment 4]

[Document name to be amended] Statement

[Correction target item name] 0069

[Correction method] Change

[Correction contents]

Further, the pipes 20 and 2 between the packed tower groups described above are used.
1 is connected to a liquid extracting means for extracting a liquid of a fraction containing a predetermined component from the end (end portion) of each unit packed column to the outside of the circulation system. That is, each of the pipes 20 and 21 between the unit packed towers is provided with a discharge valve 1A to 10 for a component having a low adsorptivity to an adsorbent (hereinafter referred to as “A-class liquid”).
A common section A liquid withdrawal pipe 12 is connected via A. Similarly, each of the pipes 20 and 21 between the unit packed towers is provided with a component having a high adsorptivity to the adsorbent (hereinafter referred to as “C
A common C-separated liquid extraction pipe 14 is connected via extraction valves 1C to 10C for "separated liquid").

[Procedure amendment 5]

[Document name to be amended] Statement

[Correction target item name] Brief description of drawings

[Correction method] Change

[Correction contents]

[Brief description of the drawings]

FIG. 1 is a first embodiment of a simulated moving bed type chromatographic separator for chromatographically separating and recovering three components contained in a raw material liquid.
FIG.

FIG. 2 is a second embodiment of a simulated moving bed type chromatographic separator for chromatographically separating and recovering two components contained in a raw material liquid.
FIG.

[Description of Signs] 1 to 10: Unit packed tower 1A to 10A: Extraction valve for A-class liquid 5B: Extraction valve for B-class liquid 1C to 10C: Extraction valve for C-class liquid 1D to 10D: Desorption liquid supply valve 1F , 3F, 5F, 7F, 9F, f: Raw material liquid supply valve A: A-class liquid (liquid with high content of component flowing out first) B: B-class liquid (content of component flowing out in the middle is high Liquid) C: C-class liquid (liquid with a high content of the last component flowing out) D: Desorption liquid F: Raw material liquid Z: Shut-off valve 12: A-group liquid extraction pipe 13: B-group liquid extraction pipe 14 : Category liquid extraction pipe 15: Raw material supply pump 16: Desorption liquid supply pump 19: Circulation pump 20,21: Pipe 30: Raw material supply pipe 31: Desorption liquid supply pipe

[Procedure amendment 6]

[Document name to be amended] Drawing

[Correction target item name] Figure 2

[Correction method] Change

[Correction contents]

FIG. 2

──────────────────────────────────────────────────続 き Continued on the front page (51) Int.Cl. ⁷ Identification symbol FI Theme coat ゛ (Reference) // G01N 30/88 G01N 30/88 N

Claims (13)

[Claims] 1. A unit packed bed of an adsorbent, through which a raw material liquid containing two or more components having different adsorbing properties to the adsorbent is passed, wherein at least one of the adsorbents has a relatively small solvent holding capacity. A unit packed bed and a plurality of unit packed beds packed with an adsorbent having a relatively large solvent holding capacity are connected so as to form a closed loop in which liquid flows endlessly over these unit packed beds, and the closed loop is connected to the unit packed bed. For the system, an operation of supplying a raw material liquid to a unit packed bed filled with an adsorbent having a relatively small solvent holding capacity, an operation of supplying a desorbed liquid to any of the unit packed beds, and a pump A flow of the raw material liquid and the desorbed liquid in one direction through the endless closed loop system to remove components having different adsorbing properties contained in the raw material liquid supplied into the closed loop system. In the direction of the liquid flow The enriched fraction liquid of the enriched component is mass-balanced with the supply of the raw material liquid and / or the desorbed liquid from a unit packed bed in which the enriched fraction of each component is present. A method for separating a plurality of components contained in a liquid, wherein the operation is performed while extracting the liquid from a closed loop. 2. One or more unit packed beds filled with an adsorbent having a relatively large solvent holding capacity are connected downstream of liquid flow of a unit packed bed filled with an adsorbent having a relatively small solvent holding capacity. The method for separating a plurality of components contained in a liquid according to claim 1, wherein: 3. The closed loop system comprises one of a unit packed bed packed with an adsorbent having a relatively small solvent holding capacity;
A plurality of unit packed beds filled with an adsorbent with a relatively large solvent holding capacity are connected endlessly, and the raw material liquid is supplied to the unit packed bed filled with an adsorbent with a relatively small solvent holding capacity. A step of extracting the fractionated liquid of the enriched component out of the closed loop while stopping the supply of the raw material liquid to the unit packed bed, and the desorbed liquid to any of the other unit packed beds 2. The method for separating a plurality of components contained in a liquid according to claim 1, wherein the step of extracting a fractionated liquid of the enriched component out of a closed loop while supplying the liquid. 4. The step of extracting the enriched component fraction liquid out of a closed loop while supplying the desorbing liquid to any one of the unit packed beds, comprises the steps of: 4. The method for separating a plurality of components contained in a liquid according to claim 3, further comprising an operation of switching a position for extracting a fraction liquid to a unit packed bed on a downstream side of a liquid flow every predetermined time. 5. The closed-loop system has two or more unit packed beds packed with an adsorbent having a relatively small solvent holding capacity and a solvent holding capacity arranged downstream of each of these unit packed beds. Enriched while supplying raw material liquid to a unit packed bed filled with an adsorbent with relatively small solvent holding capacity by connecting one or more unit packed beds filled with a large adsorbent to the unit endlessly Performing the operation of extracting the fractionated liquid of the separated component out of the closed loop, and stopping the supply of the raw material liquid to the unit packed bed filled with the adsorbent having a relatively small solvent holding capacity; and Extracting the enriched component fraction liquid out of the closed loop while supplying the desorbing liquid to the unit packed bed of Performs the process of supplying the raw material liquid to the unit packed bed After that, the supply and withdrawal positions of the liquid are sequentially switched over time to the unit packed bed on the downstream side of the liquid flow, and the raw material to the unit packed bed filled with the adsorbent having a relatively small solvent holding capacity is again used. 2. The method for separating a plurality of components contained in a liquid according to claim 1, wherein a cycle until the supply of the liquid is started is repeated as one cycle. 6. An operation of supplying a desorbing liquid to another unit packed bed in parallel with the operation of supplying a raw material liquid to a unit packed bed filled with an adsorbent having a relatively small solvent holding capacity. The method for separating a plurality of components contained in a liquid according to any one of claims 1 to 5, characterized in that: 7. The adsorbent having a relatively small solvent holding capacity is a strongly acidic cation exchange resin having a solvent holding capacity of 45% to 50%, and the adsorbent having a relatively large solvent holding capacity has a solvent holding capacity of 51%. The method for separating a plurality of components contained in a liquid according to any one of claims 1 to 5, wherein the resin is a strongly acidic cation exchange resin having a concentration of from 60% to 60%. 8. A plurality of unit packing beds filled with an adsorbent through which a raw material liquid containing two or more components having different adsorbing properties to the adsorbent are passed, and the adsorbent having a relatively small solvent holding capacity is filled. A closed loop system in which at least one of the unit packed beds and a plurality of unit packed beds filled with an adsorbent having a relatively large solvent holding capacity are connected so that liquid flows endlessly across these unit packed beds. And a raw material liquid supply means connected to supply a raw material liquid to a unit packed bed filled with a relatively small adsorbent having a solvent holding capacity in the system, and selecting one of the unit packed beds. A desorbing liquid supply means for supplying a desorbing liquid, a pump means for flowing the liquid in one direction in a closed loop system, and a component contained in the raw material liquid due to a difference in adsorptivity due to the flow of the liquid. When separation and enrichment occur in the direction of liquid flow A liquid extraction means for extracting a fraction liquid of the component from the unit packed bed in which the enriched component fraction is present to outside the closed loop, wherein a plurality of components contained in the liquid are provided. Device to separate. 9. The apparatus for separating a plurality of components contained in a liquid according to claim 8, wherein the liquid extracting unit has a discharging unit for each component contained in the raw material liquid. 10. The raw material liquid supply means has a supply / stop switching means for switching supply / stop of a raw material liquid to a unit packed bed filled with an adsorbent having a relatively small solvent holding capacity. An apparatus for separating a plurality of components contained in a liquid according to claim 8. 11. The desorbed liquid supply means has a supply position switching means for sequentially switching a supply position for a closed loop system to a unit packed bed on the downstream side of the liquid flow. An apparatus for separating a plurality of components contained in a liquid according to any one of 10 above. 12. The liquid discharging means has a discharging position switching means for switching a discharging position from a closed loop system to a unit packed bed on a downstream side of a liquid flow. An apparatus for separating a plurality of components contained in a liquid according to any one of the above. 13. The adsorbent having a relatively small solvent holding capacity is a strongly acidic cation exchange resin having a solvent holding capacity of 45% to 50%, and the adsorbent having a relatively large solvent holding capacity is a solvent holding capacity of 55%. The apparatus for separating a plurality of components contained in a liquid according to any one of claims 8 to 12, characterized in that the resin is a strongly acidic cation exchange resin having a concentration of 60% to 60%.