KR101467670B1 - Apparatus and method for improving the separation performance by simulated moving bed with backfill of product - Google Patents

Abstract

The present invention provides a method for re-injecting a product discharged from a discharge port selected for separation, a raffinate discharge port, a desorbent inlet port, an extract discharge port, and at least one discharge port selected from the raffinate discharge port and the extract discharge port, A port unit including a re-injection port;
A chromatographic unit including a chromatographic section for connecting two mutually adjacent ports; And
And a valve unit including at least one valve for controlling the movement of each of the ports at a predetermined time,
In the present invention, the efficiency of the separation process including the purity of the final product can be improved by re-injecting a part of the product through the product re-injection port.

Description

Technical Field [0001] The present invention relates to an adsorptive separation apparatus and a separation method for a moving bed adsorption separation apparatus having a product re-

The present invention relates to a sorbent separation and separation method for a similar mobile layer (SMB), and more specifically, by adding a product re-injection port, a part of the product is injected again into a similar mobile layer (SMB) (SMB) adsorbing and separating apparatus and a separating method which can be applied to the adsorbent.

The adsorption separation method is an easy separation method for securing the stability of the material because there is no phase change during the separation process.

Among these adsorption separation methods, a chromatographic separation method is widely used as a liquid adsorption separation method. Among them, the simulated moving bed (SMB) is a separation technique proposed in US Pat. No. 2,985,589 in 1961, in which a plurality of columns are continuously separated to obtain purity and stability It has an advantage of being excellent in productivity and capable of using a small amount of solvent.

FIG. 1 shows a flow chart of a conventional adsorption / separation apparatus for a similar moving bed (SMB). A typical similar moving bed (SMB) adsorption separation apparatus comprises four sections consisting of one or more columns and a desorbent inlet port located between the respective sections, an extract outlet port which is a strong adsorbate, ) Inlet port and a raffinate outlet port which is a weakly adsorbent material.

A mobile phase fluid (eluent) is used as the desorbent, which can be injected into the desorbent inlet port between section IV and section I. The fluid mixture to be separated can also be injected into the inlet port of the mixture to be separated between sections II and III. The mixture injected into the SMB adsorptive separation apparatus is separated according to the size of the interaction with the adsorbent passing through the section III according to the movement of the mobile phase fluid and the weakly adsorbed raffinate is separated from the adsorbent III.

In the SMB adsorption / separation step, all of the inflow and outflow ports are moved in the direction of movement of the mobile phase fluid, and the countercurrent effect between the mobile phase fluid and the fixed phase liquid, such as the movement of each column in the direction opposite to the movement direction of the mobile phase fluid, In this case, the movement of each port is called a switch, and the time interval between each switch is called a switch time (t _SW ) or a switching period.

The switch time (or switching interval) is set so that each port can travel at a median rate of the rate at which the raffinate and the extract pass through the adsorbent, so that the raffinate is moved from the mixture injection port to the direction of fluid movement, The extract is slowly moved in the opposite direction. The fast raffinate material is obtained as a product through a raffinate outlet port located between section III and IV through section III and the extractive material as a strong adsorbent is moved to section I and desorbed by a mobile phase fluid, And is obtained as a product at the outlet port between Extension I and Extension II.

As described above, the adsorption / separation process for the similar mobile layer (SMB) is a process in which the separation target mixture is injected and the raffinate and the extract are continuously produced.

FIG. 2 shows the concentration gradient in the two product ports over time in one switching period when a cyclic steady state is reached in the typical SMB adsorption separation process shown in FIG. Specifically, Figures 2 (a) and 2 (b) show concentration gradients at the extract outlet port and the raffinate outlet port, respectively.

2 (a), most of the raffinate material, which is an impurity, comes out from the front half of the switching section, and in the raffinate outlet port of Fig. 2 (b), most of the extract material, It is coming out later in the hour. As described above, the impurities discharged from the extract outlet port to the rear half of the switching section in the front half of the switching section and the raffinate outlet port are factors that lower the separation efficiency of the general SMB adsorptive separation apparatus.

In recent years, separation of optical isomers having similar physicochemical properties is required in the field of fine chemicals and pharmacy, and the separation efficiency is required to be increased.

In the present invention, a product of high purity can be obtained by re-injecting a part of the product discharged from the similar mobile layer (SMB) adsorption / separation step using a product re-injection port, and a similar moving layer SMB) adsorption separation apparatus and separation method.

In the present invention, at least one product for re-injecting a product discharged from a separation object mixture inlet port, a raffinate outlet port, a desorbent inlet port, an extract outlet port, and at least one outlet port selected from the raffinate outlet port and the extract outlet port A port unit including a re-injection port;

A chromatographic unit including a chromatographic section for connecting two mutually adjacent ports; And

And a valve unit including at least one valve for controlling the movement of each of the ports at predetermined time intervals.

Also, in the present invention, it is preferable to include a valve for controlling the movement of each port at a set time, a chromatographic section for connecting the separation target mixture inlet port, the raffinate outlet port, the desorbent inlet port, the extract outlet port, Wherein the adsorbent is adsorbed on the adsorbent layer,

Refining the product discharged from at least one discharge port selected from a raffinate discharge port and an extract discharge port.

In the method of separating a mixture according to the present invention, the purity of the product can be maximized by re-injecting a part of the product through the product re-injection port, and the separation efficiency of the SMB separator can be maximized.

In addition, the flow rate of each section is readjusted by the product re-injection port, thereby improving the purity of the product.

1 is a conceptual diagram showing a conventional method of operating a similar adsorption / separation layer (SMB) adsorption / separation apparatus.
FIG. 2 is a graph showing the concentration gradient at each port in the operation method of the SMB adsorption separation apparatus shown in FIG. 1, wherein the concentration gradient (a) at the extract outlet port and the concentration gradient (b) at the raffinate outlet port, .
FIG. 3 and FIG. 4 are conceptual diagrams showing a similar mobile layer (SMB) adsorption / separation apparatus and a method of operating the separation apparatus according to an embodiment of the present invention.

The present invention provides a method for re-injecting a product discharged from a discharge port selected for separation, a raffinate discharge port, a desorbent inlet port, an extract discharge port, and at least one discharge port selected from the raffinate discharge port and the extract discharge port, A port unit including a re-injection port;

A chromatographic unit including a chromatographic section for connecting two mutually adjacent ports; And

And a valve unit including at least one valve for controlling the movement of each of the ports at predetermined time intervals.

Hereinafter, the adsorption-desorption device for the like moving bed (SMB) according to the present invention will be described in more detail.

In a similar moving bed (SMB) adsorption separation apparatus of the present invention, the port unit is composed of a separation subject mixture inlet port, a raffinate outlet port, a desorbent inlet port, an extract outlet port, and a product re-inlet port. In the product re-injection port, re-injection of the product discharged from one or more discharge ports selected from a raffinate discharge port and an extract discharge port is performed, and one or more, specifically two product re- have.

The chromatographic unit in the similar mobile bed (SMB) adsorption separation apparatus of the present invention includes a chromatographic section, which connects two adjacent ports. The number of chromatographic sections is not particularly limited and may be 4 or more, specifically 4 to 7.

Typical similar moving bed (SMB) adsorbing and separating devices have three to five chromatographic sections, which may have an open loop when there are three chromatographic sections and a closed loop when there are four to five chromatographic sections. In the present invention, since a product re-injection port is formed in a general SMB device, when the number of chromatographic segments is four to five, the separation device may have an open loop. When the number of segments is 5 to 7, Lt; RTI ID = 0.0 > closed loop. ≪ / RTI >

The chromatographic section may comprise at least one chromatographic column, and may in particular comprise from 1 to 5, more particularly from 1 to 2 chromatographic columns.

In the separation apparatus according to the present invention, the valve unit includes at least one valve, and the valve controls the movement of each port at the set total switch time. Thus, in the separation apparatus according to the present invention, it is possible to simulate the countercurrent flow of the fixed phase with respect to the movement of the fluid. In addition, the valve used in the present invention may control the re-injection time of the product re-injected into the product re-injection port or select the type of the product to be re-injected. The type of the valve is not particularly limited as long as it is a valve commonly used in this field. Specifically, a rotary valve, a multi-directional valve, a multifunctional valve, and an on-off valve can be used.

In the present invention, the product re-injection port serves to reinject products discharged from one or more discharge ports selected from the raffinate discharge port and the extract discharge port, as described above.

The formation position of the product re-injection port is not particularly limited and may be formed between the extraction port and the separation port.

The product re-injection port formed between the extract outlet port and the separation object inlet port may be re-injected with the product discharged from the extract outlet port. In this case, the product re-injection port may be referred to as an extract product re-injection port.

Also, the product re-injection port may be formed between the raffinate outlet port and the separation subject mixture inlet port. The product re-injection port formed between the raffinate outlet port and the separation subject compound inlet port can be re-injected with the product discharged from the raffinate outlet port, wherein the product re- have.

Specifically, the product re-injection port of the present invention comprises: a port between an extract outlet port and a separation object mixture inlet port; And between the raffinate discharge port and the separation target mixture inlet port. In the product re-injection port formed between the extract outlet port and the separation-object mixture inlet port, the product discharged from the extract outlet port is re-injected. In the product re-injection port formed between the raffinate outlet port and the separation- The product discharged from the discharge port can be re-injected.

The present invention may further include a pump for supplying the product to the product re-injection port. In addition, the valve connected to the product re-injection port may regulate the re-injection time of the re-injected product or select the type of product to be re-injected.

In addition, the present invention is characterized by including a valve for controlling the movement of each port at a set time, a chromatographic section for connecting a separation target mixture inlet port, a raffinate outlet port, a desorbent inlet port, an extract outlet port, Wherein the adsorbent is adsorbed on the adsorbent layer,

A raffinate outlet port, and an extract outlet port. The present invention also relates to a method of separating a mixture comprising the steps of:

Hereinafter, the separation method of the mixture according to the present invention will be described in more detail.

The similar moving bed (SMB) adsorbing and separating apparatus used in the separation method of the present invention may be the above-described similar moving bed (SMB) adsorbing and separating apparatus.

In the present invention, reintroduction of the product discharged at one or more discharge ports selected from the raffinate discharge port and the extract discharge port can be effected through the product re-injection port.

Specifically, the step of re-injecting the product may include re-injecting a portion of the product discharged from the extract discharge port into the extract product re-injection port; And

And re-injecting a portion of the product discharged from the raffinate outlet port into the raffinate product re-injection port.

At this time, the extract product re-injection port is formed between the extract outlet port and the separation subject mixture inlet port, and the raffinate product re-injection port can be formed between the raffinate outlet port and the separation subject mixture inlet port.

Entrainment of product through the product re-injection port can be reused for a set reuse time of the entire switch time. Specifically, the re-entry of the product may be performed for a part or all of the total switch time, and more specifically, 10% or more, specifically 20% or more, more specifically 30 % Or more can be performed.

In particular, when using both the extract product re-injection port and the raffinate product re-injection port, re-entry of the product can be performed using both product re-injection ports simultaneously, or alternatively using two re-injection ports.

The content of the product re-injected through the product re-injection port is not particularly limited, and is preferably 5 to 80 wt%, more preferably 10 to 80 wt% of the amount of the mixture to be separated and the product to be introduced into the similar moving bed adsorption- To 60 wt%. If the amount of re-injection is less than 5 wt%, the amount of reinjection of the product is small and the re-injection effect may be insufficient. If the amount of re-injection is less than 80 wt% Productivity may be reduced.

When the product re-injection port and the raffinate product re-injection port are used together as the product re-injection port, the contents of the product re-injected into each re-injection port are respectively inputted to the similar mobile layer adsorption / 5 to 45%, specifically 10 to 30 wt%, of the input amount of the mixture and product to be separated.

The kind of the mixture to be separated in the present invention is not particularly limited, and it is preferable that the mixture contains a substance which is difficult to be separated (low selectivity substance) such as aromatic hydrocarbon or racemic mixture.

The present invention also relates to a method for producing a mixture comprising a mixture inlet port for separation, a raffinate outlet port, a desorbent inlet port, an extract outlet port, a raffinate product material inlet port for re-injecting the product discharged from the raffinate outlet port, A port unit including an extract product re-injection port for re-injecting the product;

A chromatographic unit comprising six chromatographic sections each connecting two ports adjacent to each other; And

And a valve unit including at least one valve for controlling the movement of each of the ports at predetermined time intervals.

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS Hereinafter, a method of separating a mixture using a similar mobile bed (SMB) adsorption separation apparatus according to an embodiment of the present invention will be described in detail with reference to the accompanying drawings. BRIEF DESCRIPTION OF THE DRAWINGS The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this application, illustrate embodiments of the invention and, together with the description, serve to explain the principles of the invention.

The separation method of the mixture using the adsorption and separation apparatus of the similar moving bed (SMB) according to the present invention can be applied to the separation of the aromatic hydrocarbon mixture, the ethylbenzene separation process, the chiral compound separation process, And the separation process of the racemic mixed medicines as an intermediate.

FIG. 1 shows a general SMB adsorber and separation unit. In the operation method using the separation unit, four sections play different roles. Particularly, the sections II and III are separation areas, and the raffinate (A, raffinate), which is a substance having weak adsorption power among the materials injected through the inlet port for separation between the sections II and III, moves along the moving- The extract (B, extract), which is a strong adsorbing substance, is adsorbed by the adsorbent, and the column is moved in a direction opposite to the movement of the fluid relative to the predetermined switch time interval. Therefore, And is desorbed along the mobile phase fluid as a desorbent and discharged to the extract outlet port. In addition, the sections I and IV are regeneration zones, and the raffinate (A), which has not been discharged from the raffinate outlet port, is adsorbed to the raffinate (A) to be adsorbed to regenerate the desorbent. In the section I, (B) is detached and thus the stationary phase is regenerated.

FIG. 2 is a graph showing the concentration gradient at each product outlet port of a typical similar mobile bed (SMB) adsorption separation process. In the concentration gradient of the extract outlet port (FIG. 2 (a)), Most of the raffinate material is in the first half of the switch time and in the concentration gradient at the raffinate outlet port (Figure 2 (b)), most of the extract material, which is an impurity, It is present in the latter half of the switch time.

As shown in FIG. 2, in order to reduce the impurities in the extract and the raffinate outlet port, the content of the raffinate material present in the section II and the extract material present in the section III must be reduced.

3 and 4 are conceptual diagrams of a similar mobile bed (SMB) adsorption / separation apparatus according to an embodiment of the present invention and a conceptual diagram showing a method of operating the separation apparatus.

The SMB separator according to Fig. 3 comprises a feed inlet port, a raffinate outlet port, a desorbent inlet port, an extract outlet port, a product re-inlet port 1 (an extract product re- , A product re-injection port 2 (re-inflation product re-injection port), six chromatographic sections (closed loop) connecting two adjacent ports, and a valve for controlling the movement of each port do. In the above chromatography section, two chromatographic columns are arranged for sections I and IV, and one chromatography column is arranged for sections II-1, II-2, III-1 and III-2.

The separation device according to an embodiment of the present invention has a product re-injection port between section II-1 and II-2 and between sections III-1 and III-2, Such as a pump and a valve, for injecting a part or all of the liquid.

Sections I and IV play the same role as the general SMB sorbent separator described above. Section II in a typical similar moving bed (SMB) sorbent separator is divided into sections II-1 and II-2 in the embodiment of the present invention by adding product re-injection port 1. The fraction II-2 has a larger flow rate than the fraction II-1 because part of the product of the extract is injected through the product re-injection port 1. The fraction II-1 and the fraction II- There is more extract material than in section II of the device separation method.

In addition, section III in the general adsorptive separation layer (SMB) is divided into sections III-1 and III-2 as product re-injection port 2 is added. Part of the raffinate product is injected through product re-injection port 2, so that Ⅲ-2 has a larger flow rate than that of segment III-1, while a similar similar mobile layer (SMB) adsorption is carried out in segments III- There are more raffinate materials than in Region III in the separator separation method.

At this time, it is preferable that the flow rate of the mixture injection port is reduced by the additional injection flow rate because the product injection port 1 and the product re-injection port 2 cause additional injection flow. Therefore, the flow rate of II-2 in the embodiment of the present invention is larger than the flow rate of the section II in the separation method of a general similar mobile bed (SMB) adsorption separation apparatus, The flow rate of III-1 in the embodiment of the present invention becomes smaller than the flow rate of the section III in the separation method. In addition, if the flow rate of the mixture injection port for separation is reduced, productivity may be deteriorated. Therefore, it is preferable to increase the concentration of the crude mixture.

The method of separating the mixture using the SMB device according to the present invention differs from the conventional SMB separation method in the following points.

A portion of the raffinate product is injected through a product re-injection port located between the mixture injection port and the raffinate exit port during some or all of one switching period, and a portion of the product of the product is placed between the mixture inlet port and the extract outlet port Injected through the re-injection port.

Specifically, first, it is the presence of product re-injection port. Unlike a typical similar mobile bed sorbent sorbent sorbent sorbent, the sorbent sorbent sorbent sorbent sorbent sorbent sorbent sorbent sorbent sorbent sorbent sorbent sorbent sorbent sorbent sorbent sorbent sorbent sorbent sorbent sorbent sorbate sorbate sorbate sorbate sorbate sorbate

Second, product re-injection through the product re-injection port is achieved. A portion of the product of the extract is injected through the product re-injection port adjacent to the extract outlet port to contribute to the enhancement of the purity of the extract, and a portion of the raffinate product is injected through the product re-injection port adjacent to the raffinate outlet port, .

Third, there is a difference in flow rate caused by re-injection of product through the product re-injection port. The flow rate of the section II-2 of the separation apparatus of the present embodiment becomes large (see FIGS. 1 and 3) as compared with the flow rate of the general similar moving bed (SMB) separation apparatus of section II, It accelerates the transport of Nate materials and helps to improve the purity of the extract. Also, the flow rate in section III-1 of the separator of this embodiment is smaller than the flow rate in section III of a general similar mobile bed (SMB) separator, which slows the movement of the impurities, which are impurities in the raffinate product This will help improve raffinate purity.

Example

The similar moving bed (SMB) adsorption separation apparatus according to this embodiment is designed to have six chromatographic sections (closed loop) and two product re-injection ports as shown in FIG. Simulation studies were conducted to confirm the improved performance of the separation of the mixture using the separator.

The operation method of the process was designed in three ways, and it is hereinafter referred to as Test Example 1, Test Example 2 and Test Example 3 separately.

In Test Example 1, the extract product was injected through the product re-injection port 1 and the raffinate product was injected through the product re-injection port 2 during the entire switching period.

In Test Example 2, the extract product was injected through the product re-injection port 1 during the first half of the switching period and the raffinate product was injected through the product re-injection port 2 during the latter half.

In Test Example 3, the raffinate product was injected through the product re-injection port 2 during the first half of the switching period and the product product was injected through the product re-injection port 1 during the latter half.

In the above-described Test Examples 1 to 3, the process of re-injecting all the raffinate and extract products was designed. However, it is also possible to design a process of re-injecting only one of the two products.

Although the separation target material in this embodiment sets a virtual substance having a selectivity of 1.5, the separation process using the present invention is not limited to this, and the separation process of the mixture of aromatic hydrocarbons, the separation process of ethylbenzene, Separation process of chiral compounds, and the like, and can be applied to the separation process of racemic mixed medicines, which are final products or intermediates during the manufacture of medicines.

As a comparative example, a typical similar mobile bed (SMB) adsorptive separation process consisting of four closure loops with two chromatographic columns per section was used for comparison between processes using the same adsorbent amount.

In this experiment and comparative example, gPROMS Modelbuilder which is a commercial process simulation program was used and the separation performance of each process was compared with three performance indexes of purity, recovery and solvent consumption (eluent consumption) .

In order to simulate the processes of the above Experimental Examples and Comparative Examples, a node model for modeling the adsorption and separation behavior of each component in the column and a model for the adsorption separation process of the similar mobile layer (SMB) is required.

The column model used a transport-dispersive model. The model equations are based on differential mass balance equations, LDF linear driving force model equations and equilibrium isotherm, initial and boundary conditions for each material, conditions. In addition, the node model is composed of the material quantities, which relate to the fluid mixture (feed), desorbent, product re-injection, and product discharge flow, depending on the role of each port.

In the Examples and Comparative Examples of the similar mobile layer (SMB) adsorption separation step having the general similar mobile layer (SMB) adsorption separation step and the product material injection step using the mathematical model equations, the system shown in Table 1 and Table 2 Process simulation was performed using process variables.

Typical SMB Process Comparison Example SMB system parameters SMB configuration 2-2-2-2 (8 column) D (column diameter) (cm) One L (column length) (cm) 10 ε (total porosity) 0.4 N _disp (the number of dispersion units) 80 mass transfer coefficient k (both components) (1 / s) 0.5 Isotherm coefficient _{K A (raffinate component) (-} ) 2 K _B (extract component) (-) 3 b _A (raffinate component) (L / g) 0.06 b _B (extract component) (L / g) 0.08 Operating parameters C _{i , F} (feed concentration) i = A, B (g / L) 3 Q _F (feed flowrate) (ml / min) 3.18 Q _E (extract flowrate) (ml / min) 11.04 Q _R (raffinate flowrate) (ml / min) 5.45 Q _D (desorbent flowrate) (ml / min) 13.31 Q ₁ (flowrate of zone ₁ ) (ml / min) 30.00 Q ₂ (flowrate of zone ₂ ) (ml / min) 18.96 Q ₃ (flowrate of zone ₃ ) (ml / min) 22.13 Q ₄ (flowrate of zone ₄ ) (ml / min) 16.69 T _sw (switching time) (ml / min) 37.38

SMB process example with recharging SMB system parameters SMB configuration 2-1-1-1-1-2 (8 column) D (column diameter) (cm) One L (column length) (cm) 10 ε (total porosity) 0.4 N _disp (the number of dispersion units) 80 mass transfer coefficient k (both components) (1 / s) 0.5 Isotherm coefficient _{K A (raffinate component) (-} ) 2 K _B (extract component) (-) 3 b _A (raffinate component) (L / g) 0.06 b _B (extract component) (L / g) 0.08 Operating parameters C _{i , F} (feed concentration) i = A, B (g / L) 5 Total Q _F (total feed flowrate) (ml / min) 3.18 Q _E (extract flowrate) (ml / min) 11.04 Q _R (raffinate flowrate) (ml / min) 5.45 Q _D (desorbent flowrate) (ml / min) 13.31 Q ₁ (flowrate of zone ₁ ) (ml / min) 30.00 Q _{2 -1} (flowrate of zone _{2 - 1} ) (ml / min) 18.96 Q _{3 -2} (flowrate of zone _{3 - 2} ) (ml / min) 22.13 Q ₄ (flowrate of zone ₄ ) (ml / min) 16.69 Backfill ratio (-) 0.2 T _sw (switching time) (ml / min) 37.38

The backfill ratio in Table 2 indicates the amount of product re-injected in the total feed amount in a volume ratio in the SMB adsorption separation process including the product re-injection step, for example, The re-injection rate of 0.2 means re-injecting the extract and raffinate product, respectively, of an amount corresponding to 20% of the total mixture injection volume. At this time, since the injection amount of the mixture injection port is reduced by the re-injection ratio, the crude mixture is injected in an amount corresponding to 60% of the total mixture injection amount.

In Test Example 1, the product corresponding to 20% of the total amount of the mixture was injected during the entire switching period, so that the re-injection of the product was performed at a flow rate of 0.64 ml / min, which is 20% of the total feed flow rate The inlet of the crude mixture is made up of the mixture inlet port at a flow rate of 1.91 ml / min, corresponding to 60% of the remaining total mixture inlet flow rate.

In Test Example 2, the product corresponding to 20% of the total amount of the mixture is injected for half the time of the switching section. Therefore, at the flow rate of 1.27 ml / min, which is 40% of the total feed flow rate, In the latter half of the switching section, the raffinate product is re-injected at the product re-injection port 2, and at a flow rate of 1.91 ml / min corresponding to 60% of the remaining total mixture flow rate So that the influx of the mixture is made to the mixture inlet port.

Likewise, in Test Example 3, 20% of the total amount of the mixture is injected during the half-time of the switching section. Therefore, at a flow rate of 1.27 ml / min, which is 40% of the total feed flow rate, The reintroduction of the raffinate product at the product re-injection port 2 and the re-injection of the extract product at the product re-injection port 1 at the latter half of the switching period and at a flow rate of 1.91 ml / min corresponding to 60% So that the introduction of the crude mixture takes place at the mixture inlet port.

The results of the three test examples and the comparative example are shown in Table 3. As can be seen from Table 3, the adsorption and separation process of the similar mobile layer (SMB) having the product re-injecting step according to the present invention showed better separation performance than that of the conventional mobile adsorption process in terms of purity, recovery rate, The solvent used in the mixture inlet port was reduced through product rejuvenation, and a noticeable decrease in the solvent consumption was confirmed. The purity of the extract was improved more than the raffinate in Test Example 1 and the raffinate was further improved in the Test Example 2 and Test Example 3 than the extract.

Comparative Example (Conventional Process) and Test Example Comparison Operating mode Purity [%] Recovery [%] Eluent consumption [L / g] Ext Shelf Ext Shelf Ext Shelf Comparative Example (Conventional Process) 96.6 97.8 97.8 96.6 1.77 1.79 Test Example 1 98.0 98.0 98.0 98.0 1.63 1.63 Test Example 2 97.3 98.5 98.5 97.3 1.62 1.64 Test Example 3 97.7 98.6 98.6 97.6 1.62 1.64

The preferred embodiments of the present invention described above are disclosed for illustrative purposes, and those skilled in the art will recognize that various modifications, additions and substitutions are possible within the spirit and scope of the present invention. Such modifications, alterations, and additions should be regarded as falling within the scope of the following claims.

Claims (14)

A raffinate product inlet port, a raffinate outlet port, a desorbent inlet port, an extract outlet port, a raffinate product inlet port for re-injecting the product discharged from the raffinate outlet port, and a product discharged from the extract outlet port, A port unit including an extract product re-injection port;
A chromatographic unit comprising six chromatographic sections each connecting two ports adjacent to each other; And
A valve unit including at least one valve for controlling the movement of each of the ports at a set time;
Wherein the adsorbing material is adsorbed to the adsorbent.
The method according to claim 1,
Wherein the re-injection port of the extract product is formed between the extract outlet port and the separation inlet port for separation.
delete The method according to claim 1,
Wherein the raffinate product re-injection port is formed between the raffinate outlet port and the separation subject mixture inlet port.
delete The method according to claim 1,
Wherein the extract product re-injection port is formed between the extract outlet port and the separation subject mixture inlet port and the raffinate product re-injection port is formed between the raffinate outlet port and the separation subject mixture inlet port.
The method according to claim 6,
In the product re-injection port formed between the extract outlet port and the separating object inlet port, the product discharged from the extract outlet port is re-injected,
And a product re-injection port formed between the raffinate outlet port and the separation subject mixture inlet port for re-injecting the product discharged from the raffinate outlet port.
The method according to claim 1,
A raffinate outlet port and a pump for feeding the product discharged from the extract outlet port to the product re-inlet port.
A chromatographic section for separating the mixture inlet port, the raffinate outlet port, the desorbent inlet port, the extract outlet port, the raffinate product inlet port, the extract product inlet port, and the two adjacent ports, And a valve for controlling the movement of each of the ports, the method comprising:
Re-injecting a portion of the product discharged from the extract port into the extract product re-injection port; And
And re-injecting a portion of the product discharged from the raffinate exit port into the raffinate product re-injection port.
delete 10. The method of claim 9,
The extract product re-injection port is formed between the extract outlet port and the separation subject mixture inlet port,
Wherein the raffinate product re-injection port is formed between the raffinate outlet port and the separation subject mixture inlet port.
10. The method of claim 9,
Wherein the reintroduction of the product through the reextraction port of the extract product and the reintroduction port of the raffinate product is performed during some or all of the total switch time.
10. The method of claim 9,
The content of product re-injected through the extract product re-injection port and the raffinate product re-injection port is such that the mixture to be separated to be fed into the similar mobile bed adsorber and during the entire switch time and from 5 to 80 wt% Separation method.


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