JPH1190104A - Pseude moving bed type separating device - Google Patents

Abstract

PROBLEM TO BE SOLVED: To clean a circulating fluid passage for a short time by introducing a cleaning liquid from one end part of a packed bed to clean the packed bed. SOLUTION: In the case of cleaning, for example a column (a), a t first, a pump P and PF are stopped. And a solenoid valve VDa and a solenoid valve VEa or VRa are opened and the other solenoid valves are closed. Next, a pump PD so started and the cleaning liquid is supplied to the column (a) through an eluant supply line D and an eluant introducing line and is drawn from an extract drawing line Ea or a raffinate drawing line Ra . It is judged that the cleaning of the column (a) is finished when the concentration of a strong absorption component or a weak absorption component becomes equal to or below a prescribed value in a strong absorption component concentration monitor EM provided in an extract integrated drawing line or a weak absorption component concentration monitor ER provided in a raffinate integrated drawing line R.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a simulated moving bed type separation apparatus, and more particularly to a simulated moving bed type separation apparatus provided with a packed bed washing means for washing a packed bed. The present invention relates to a simulated moving bed type separation apparatus capable of washing a packed bed in a shorter time than a bed type separation apparatus.

[0002]

2. Description of the Related Art As a simulated moving bed type separation apparatus, a circulating fluid flow path in which two or more packed beds filled with a separating filler are connected in series and endlessly by piping or the like, An eluent inlet for introducing an eluent into the circulating fluid flow path, an extract liquid outlet for extracting a solution rich in strongly adsorbed components from the circulating fluid flow path, and a raw material solution containing the component to be separated into the circulating fluid. A source solution inlet for introducing into the flow channel, a raffinate liquid outlet for extracting a solution rich in weakly adsorbed components from the circulating fluid channel, and a pump for forcibly circulating a liquid through the circulating fluid channel; Dressed,
Further, the eluent inlet, the extract outlet, the raw solution inlet, and the raffinate outlet are formed of a liquid (hereinafter, referred to as “circulating liquid”) circulating in the circulating fluid flow path. Along the circulation direction, eluent inlet,
A simulated moving bed type in which an extract liquid outlet, a raw material solution inlet, and a raffinate liquid outlet are arranged in the circulating fluid flow path in this order, and are provided so as to intermittently move while maintaining the order. Separation devices have been previously known.

[0003] The simulated moving bed type separation apparatus described above is capable of continuous operation, greatly reducing the amount of eluate compared with a batch type chromatographic separation apparatus, and obtaining an eluate having a high concentration of a target substance. It has been used for the separation and purification of various chemical products such as medicines, agricultural chemicals, fragrances and sugars.

[0004]

In the simulated moving bed type separation apparatus, when the operation of the apparatus is terminated or stopped, a washing liquid such as an eluent is caused to flow through the circulating fluid flow path and the circulating fluid flow path. It was common to perform a wash.

However, since the packed bed is connected in series to the circulating fluid flow path as described above, the pressure loss of the circulating fluid flow path is reduced by the pressure loss caused by the packed bed and the piping constituting the circulating fluid flow path. The size is the sum of all the values. Therefore,
The pressure loss when flowing the cleaning liquid through the circulating fluid flow path is extremely large, and therefore, it has been difficult to flow the cleaning liquid through the circulating fluid flow path at a high flow rate. In addition, the cleaning liquid injected into the circulating fluid flow path is discharged to the outside after passing through all the packed beds and pipes connected in series, so that the cleaning liquid is injected into the circulating fluid flow path and then discharged to the outside. It took a long time to be done. For these reasons, conventionally, it took a long time to clean the circulating fluid flow path. In addition, impurities accumulated in one packed bed
There is also a problem that the cleaning fluid circulating in the circulation fluid flow path circulates in the circulation fluid flow path and contaminates other packed beds.

[0006] It is an object of the present invention to provide a simulated moving bed type separation apparatus which solves the above-mentioned problems of the conventional simulated moving bed type separation apparatus.

[0007] Specifically, the present invention can clean the circulating fluid flow path in a short time, and when cleaning the circulating fluid flow path, impurities accumulated in one packed bed are removed by another. It is an object of the present invention to provide a simulated moving bed type separation apparatus which does not contaminate a packed bed.

[0008]

SUMMARY OF THE INVENTION A simulated moving bed type separation apparatus for solving the above-mentioned problems has the following features. (1) Two or more separation fillers connected in series and endlessly are contained therein. A circulating fluid channel having a packed bed packed therein and forcibly circulating a circulating fluid therein, an eluent inlet for introducing an eluent into the circulating fluid channel, and a component to be separated. An extract liquid outlet for extracting a solution rich in strongly adsorbed components in the raw material solution from the circulating fluid flow path, a raw material solution inlet for introducing the raw material solution into the circulating fluid flow path, and weak adsorption in the raw material solution A raffinate liquid outlet for extracting a solution rich in components from the circulating fluid flow path, and the eluent inlet, extract liquid outlet, raw material solution inlet, and raffinate liquid outlet are circulated through the circulating liquid. Eluent along the direction Inlet, extract draw-out port, feedstock introducing port is arranged in the order of raffinate draw opening,
And in the pseudo moving bed type separation apparatus provided so as to intermittently move while maintaining the order, a washing liquid for washing the inside of the packed bed is introduced from one end of each of the packed beds. And a simulated moving bed type separation apparatus characterized by comprising a packed bed washing means for washing the packed bed, and (2) one or more packed bed washing means in the above (1). The simulated moving bed type separation apparatus according to (1), which is a packed bed washing means that supplies a washing liquid for each unit, and switches a unit for supplying the washing liquid at regular intervals, with the column as one unit.

[0009]

DESCRIPTION OF THE PREFERRED EMBODIMENTS As described above, the simulated moving bed type separation apparatus of the present invention comprises (A) and (a) connected in series and endlessly,
A circulating fluid flow path having two or more packing beds filled with a separation filler therein and capable of forcibly circulating a circulating liquid therein; and (b) supplying an eluent to the circulating fluid flow path. An eluent inlet for introduction, (c) an extract liquid outlet for extracting a circulating liquid rich in strongly adsorbed components (hereinafter referred to as "extract liquid") from the circulating fluid flow path, and (d) a component to be separated. A raw material solution inlet for introducing a raw material solution into the circulating fluid flow path, and (e) a raffinate liquid outlet for extracting a circulating liquid (hereinafter, referred to as “raffinate liquid”) rich in weakly adsorbed components from the circulating fluid flow path. And (B) the eluent inlet, extract liquid outlet, raw material solution inlet, and raffinate outlet are eluted along a circulation direction of the circulating liquid circulating through the circulating fluid flow path. Liquid inlet, extract liquid outlet, raw material solution , Arranged in the order of the raffinate liquid outlet, and provided so as to intermittently move while maintaining said order, and (C) one end of each of the packed beds to be washed And a washing means for washing the inside of the packed bed by introducing a washing liquid for washing the inside of the packed bed.

[0010] Of the components contained in the raw material solution, strongly adsorbed components are relatively strongly adsorbed to the packed bed, while weakly adsorbed components are adsorbed relatively weakly to the packed bed.

1. 1. Components of the Present Invention 1.1 Circulating Fluid Channel In the simulated moving bed separator of the present invention, two or more packed beds are connected in series and endlessly to forcibly circulate the circulating liquid in one direction. A circulating fluid flow path is formed.

Examples of the circulating fluid flow path include a circulating fluid flow path in which a packed bed is connected endlessly through a pipe. The circulating fluid flow path may be provided with a fluid forced circulation means for forcibly circulating the circulating liquid in one direction.

As the fluid forced circulation means, any means having any structure and type may be used as long as the circulating liquid can be forcibly circulated in one direction. A pump or the like interposed in the device can be used. There is no particular limitation on the pump that can be interposed in the circulating fluid flow path. Specifically, any of a positive displacement pump such as a diaphragm pump and a plunger pump and a turbo pump such as a centrifugal pump can be used. Among these pumps, a positive displacement pump is used because the circulating fluid does not flow backward because valves are provided on the suction side and the discharge side of the pump, it can easily cope with high pressure, and the flow rate is accurate. Diaphragm pumps are most preferred, especially since circulating fluid does not directly contact worn parts such as pistons and plungers, so that circulating fluid is not contaminated. When a centrifugal pump is used, a check valve is preferably provided near the discharge port of the pump to prevent the circulating fluid from flowing back.

As another means, a combination of a pressure regulating valve provided in the circulating fluid flow path, which circulates the circulating fluid in one direction by adjusting a pressure balance in the circulating fluid flow path, may be used. it can.

The circulating fluid channel has an eluent inlet for introducing an eluent, an extract outlet for extracting a circulating fluid rich in strongly adsorbed components, and a raw material solution containing a mixture of components to be separated. The raw material solution inlet to be introduced, and the raffinate liquid outlet for extracting the circulating liquid rich in weakly adsorbed components,
They are provided in this order.

The eluent inlet, extract outlet, raw material inlet, and raffinate outlet are:
In a state where the order is maintained, the circulating fluid flow path is provided so as to be movable in the circulating fluid circulating direction inside the circulating fluid flow path.
An appropriate switching means such as a rotary valve and an open / close valve can be used for switching the eluent inlet, extract liquid outlet, raw material solution inlet, and raffinate liquid outlet. As the open / close valve, a pneumatically driven valve that opens and closes with pneumatic pressure, an electromagnetic valve, an electric valve, or the like can be used. The switching means such as the rotary valve and the opening / closing valve can be controlled by an appropriate control device such as a microcomputer, a personal computer, and a minicomputer, and can be switched at predetermined time intervals.

The extract liquid outlet and the raffinate liquid outlet may be provided with a flow rate control valve and a pressure control valve so that the amount of the extract liquid and the raffinate liquid to be extracted can be adjusted. Further, a predetermined amount may be extracted using a variable discharge amount type pump. Further, a variable discharge type eluent pump for supplying an eluent and a variable discharge type material solution pump for supplying a raw material solution are connected to the eluent inlet and the raw material solution inlet, respectively. By adjusting the discharge amounts of the pump and the raw material solution pump, the introduction amounts of the eluent and the raw material solution can be adjusted.
Instead of connecting a variable discharge type pump to the eluent inlet and the raw material solution inlet, a fixed displacement pump and a throttle valve may be provided respectively.

In the circulating fluid flow path, a desorption zone (IV) is formed in the packed bed between the eluent inlet and the extract outlet, and the desorption zone (IV) is formed between the extract outlet and the raw material inlet. In the packed bed
(III) is formed, a purification zone (II) is formed in the packed bed between the raw material solution inlet and the raffinate liquid outlet, and a packed bed between the raffinate liquid outlet and the eluent inlet is formed in the packed bed. An adsorption zone (I) is formed.

In the desorption zone (IV), the eluent introduced from the eluent inlet port flows through the packed bed together with the circulating liquid. When the eluent comes into contact with the separation filler, the strongly adsorbed component that has been adsorbed on the separation filler is desorbed from the filler, and the strongly adsorbed component is extracted as an extract liquid from the extract liquid outlet. In the part immediately after the eluent introduction port in the desorption zone (IV), the concentration of the strongly adsorbed component in the circulating liquid is substantially close to 0, and the circulating liquid in the desorption zone (IV) along the traveling direction of the circulating liquid. The concentration of the strongly adsorbed components in it increases.

In the concentration zone (III), the strongly adsorbed components in the circulating liquid are adsorbed by the separation filler, and the weakly adsorbed components are desorbed from the filler.

In the refining zone (II), the strongly adsorbed component and the weakly adsorbed component in the raw material solution introduced from the raw material solution inlet are:
The concentration of the strongly adsorbed component in the circulating liquid in the region from the raw material solution inlet to the raffinate liquid outlet is substantially zero, and the raffinate liquid outlet is separated. , A raffinate solution containing a weakly adsorbed component is extracted.

In the adsorption zone (I), the weakly adsorbed component is adsorbed on the separating filler, and the concentration of the weakly adsorbed component in the circulating liquid decreases to substantially zero. Therefore, the circulating liquid containing only the eluent substantially containing neither the weakly adsorbed component nor the strongly adsorbed component flows out of the adsorption zone (I) and enters the desorption zone (IV).

The desorption zone (I) is switched by switching the eluent inlet, extract outlet, raw material inlet, and raffinate outlet at regular intervals.
V), the concentration zone (III), the purification zone (II), and the adsorption zone (I) move on the circulation fluid flow path, respectively.

1.2 Packed Bed The number of packed beds included in the circulating fluid flow path is not particularly limited as long as it is two or more.
The desorption zone (IV), the concentration zone (III), the purification zone (I
The number of packed beds is preferably 4, 6, 8, 10, 12, or 24, since I) and the adsorption zone (I) are formed.

As the packed bed forming the circulating fluid flow path, for example, a column filled with a separating packing material can be used.

1.2.1 Packing Material for Separation The column contains packing material for separation capable of adsorbing the component to be separated.

Examples of the packing for separation include packings for liquid chromatography such as normal-phase packings and packings for reversed-phase packing. Particularly preferred examples include packings for high-performance liquid chromatography.

Various known isomer separation fillers can be used as the separation filler depending on the component to be separated.

For example, if an optical isomer is to be separated, an optically active polymer compound and an optically resolving filler utilizing a low molecular compound having an optical resolving ability can be used as the separating filler. . Examples of the filler for optical resolution using the optically active polymer compound include a filler in which a polysaccharide derivative (such as an ester or carbamate of cellulose or amylose), a polyacrylate derivative, or a polyamide derivative is supported on silica gel or the like, silica gel And a bead-type filler obtained by granulating the polymer itself without using a polymer, and a cross-linkable filler obtained by further cross-linking the polymer. In addition, as a filler for optical resolution utilizing a low molecular compound having optical resolution ability, for example, an amino acid or a derivative thereof, a crown ether or a derivative thereof, a low molecular compound having an optical resolution ability such as cyclodextrin or a derivative thereof, Silica gel, alumina, zirconia,
A filler for optical resolution supported on an inorganic carrier such as titanium oxide, silicate, or diatomaceous earth, or an organic carrier such as polyurethane, polystyrene, or a polyacrylic acid derivative can be given.

Commercially available fillers for optical resolution can be used, and CHIRALCEL manufactured by Daicel Chemical Industries, Ltd. can be used.
OB (registered trademark), CHIRALCEL OD (registered trademark), CROWNPAK
CR (+) (registered trademark), CHIRALCEL CA-1 (registered trademark), C
HIRALCEL OA (registered trademark), CHIRALCEL OK (registered trademark), CHIRALCEL OJ (registered trademark), CHIRALCEL OC (registered trademark), CHIRALCEL OF (registered trademark), CHIRALCEL OG (registered trademark), CHIRALCEL WH (registered trademark), CHIRALPAK WM
(Registered trademark), CHIRALPAK WE (registered trademark), CHIRAL-PAK
OT (+) (registered trademark), CHIRALPAK OP (+) (registered trademark), CHIRALPAK AS (registered trademark), CHIRALPAK AD (registered trademark), CHIRALCEL OJ-R (registered trademark), CHIRALCELOD-R
(Registered trademark) can be mentioned as a suitable example.

When isomerized saccharides including oligosaccharides are separated into fructose and glucose, the separating filler may be:
Alkaline earth metal salts such as calcium, barium, and strontium, etc., for strongly acidic ion exchange resins, and crystallinity such as zeolite Y in which exchangeable cations are replaced with ammonium, sodium, potassium, calcium, strontium, barium, etc. Aluminosilicate or the like can be used.

As a preferable separating filler for separating fatty acid and triglyceride, a basic ion exchange resin having a skeleton of a copolymer of styrene and divinylbenzene can be mentioned. For example, ROHM
Weakly basic ion exchange resins such as Amberlite IRA 93 manufactured by Andhase and Duolite A 377 manufactured by Sumitomo Chemical Co., Ltd .; Amberlite IRA 400 manufactured by Rohm and Haas; Duo manufactured by Sumitomo Chemical Co., Ltd. Strongly basic ion exchange resins such as Light A 161 can be mentioned.

The average particle size of the separation filler packed in the column varies depending on the type of the component to be separated, the volume flow rate of the solvent flowing through each unit column, and the like. , Usually 1 to 300 µm, preferably 2 to
100 μm. However, if the pressure loss in the column forming the simulated moving bed is to be suppressed to a small value, 10 to 10
It is desirable to adjust the average particle size of the separation filler to 100 μm. When the average particle size of the separation filler is within the above range, the pressure loss in the simulated moving bed can be reduced, and for example, the pressure loss can be suppressed to 50 kgf / cm ² or less. On the other hand, the larger the average particle size of the separation filler, the lower the theoretical number of adsorption stages. Therefore, in order to achieve a practical number of theoretical plates, the average particle size of the separation filler is usually 15 to 75 μm.
m.

1.3 Eluent Examples of the eluent supplied to the circulating fluid channel include alcohols such as methanol, ethanol and isopropanol, ketones such as acetone, methyl ethyl ketone and cyclohexanone, ethyl acetate and methyl acetate. And esters such as ethyl butyrate, pentane,
Hydrocarbons such as hexane, isohexane, cyclohexane, and heptane; ethers such as diethyl ether, dibutyl ether, and diisopropyl ether; carboxylic acids such as formic acid and acetic acid; aromatic hydrocarbons such as benzene, alkylbenzene, and toluene;
Halogenated hydrocarbons such as monochlorobenzene and dichlorobenzene, amides such as dimethylformamide, nitriles such as acetonitrile and butyronitrile, pyrrolidones such as N-methylpyrrolidone, water,
And a buffer. Further, a mixture of various organic solvents such as the alcohols, ketones, and hydrocarbons, and a water-miscible organic solvent such as methanol, acetone, acetonitrile, dimethylformamide, and N-methylpyrrolidone; Mixtures with water and / or buffers can also be mentioned as eluents.

This eluent can be used as a normal phase mobile phase or a reverse phase mobile phase. Which eluent is preferable is appropriately determined according to the type of the component or compound to be separated. In addition, the eluent may contain a basic substance such as diethylamine or an acidic compound such as acetic acid as an additive, and if these additives are contained in the eluent, separation may occur. Can be improved.

1.4 Raw Material Solution The raw material solution supplied to the circulation fluid channel is not particularly limited as long as it is a multi-component mixture such as a binary mixture having a solute that needs to be separated. , Various compounds used in the fields of food, feed, flavoring, etc.,
Examples include thalidomide as a pharmaceutical, EPN as an organic phosphorus pesticide, monosodium glutamic acid as a chemical seasoning, and menthol as a flavor. Further examples include optically active alcohols, optically active amines and optically active amines. Amides and optically active esters.

The solute may be, for example, a mixture of optical isomers, a mixture of positional isomers, or a mixture of components necessary and unnecessary from a certain viewpoint.

In the present invention, the plurality of components to be separated may be, for example, a multi-component mixture of three components, four components and the like. In the case of a multi-component mixture, in order to separate the required one component using the simulated moving bed type separation device of the present invention,
The group containing the required one component is separated into two groups, a group containing the required one component and a group not containing the required component. Then, the group containing the required one component is divided into a small group containing the required one component and another group. The necessary components can be separated by repeating the operation of separating into two groups, such as a small group, and so on a predetermined number of times.

Further, a batch operation (for example, crystallization, membrane separation, batch chromatography, distillation or the like) using a separation apparatus other than the simulated moving bed separation apparatus and the simulated moving bed separation apparatus of the present invention are used. The required one component can also be separated from the multi-component mixture.

1.5 Packed Bed Washing Unit In the simulated moving bed type separation apparatus of the present invention, the packed bed washing unit has a function of introducing a washing liquid from one end of the packed bed to wash the packed bed. Have. As the cleaning solution, strongly adsorbed components, weakly adsorbed components, and other impurities,
Any liquid that can be eluted from the packing material for separation packed in the packed bed and does not strongly adsorb to the packing material for separation or alter the packing material for separation and the eluent etc. Such a liquid can also be used.

Accordingly, examples of the washing solution include alcohols such as methanol, ethanol and isopropanol, ketones such as acetone, methyl ethyl ketone and cyclohexanone, esters such as ethyl acetate, methyl acetate and ethyl butyrate, pentane, hexane and the like. And hydrocarbons such as heptane, ethers such as diethyl ether, dibutyl ether and diisopropyl ether, carboxylic acids such as formic acid and acetic acid, aromatic hydrocarbons such as benzene, alkylbenzene and toluene, monochlorobenzene and dichlorobenzene, etc. Halogenated hydrocarbons, amides such as dimethylformamide, nitriles such as acetonitrile and butyronitrile, pyrrolidones such as N-methylpyrrolidone, water, And the like can be mentioned buffer. Further, a mixture of various organic solvents such as the alcohols, ketones, and hydrocarbons, and a water-miscible organic solvent such as methanol, acetone, acetonitrile, dimethylformamide, and N-methylpyrrolidone; A mixed solution with water and / or a buffer solution can also be mentioned as the washing solution. Furthermore, a solution in which an anionic surfactant, a cationic surfactant, or a nonionic surfactant is dissolved in these liquids,
It can be mentioned as a washing liquid. Among these washing liquids, the liquid used as the eluent can be mentioned as the most preferable example.

As the packed bed washing means, for example, a washing liquid injecting means for injecting a washing liquid into the inlet of the packed bed, a washing liquid discharging means for discharging the washing liquid from the outlet side of the packed bed,
A packed bed washing means provided with a washing liquid sending means for sending a washing liquid to the washing liquid injecting means.

The cleaning liquid injection means and the cleaning liquid discharge means include a cleaning liquid injection pipe connected to the inlet side of the packed bed and a cleaning liquid discharge pipe connected to the outlet side of the packed bed. An opening / closing valve can be interposed in each of the cleaning liquid injection pipe and the cleaning liquid discharge pipe. The on-off valve interposed between the cleaning liquid injection pipe and the cleaning liquid discharge pipe is controlled by a control device that controls a switching unit that switches an eluent introduction port and the like. It is closed in the state of performing purification (hereinafter, referred to as “separation / purification mode”), and is in the state of cleaning the packed bed by the simulated moving bed type separation apparatus (hereinafter, referred to as “washing mode”). It can be controlled to be open.

Here, in the separation / purification mode, as described above, the eluent inlet, the extract outlet, the raw material inlet, and the raffinate outlet are sequentially switched so that the circulating fluid flow path By circulating the circulating liquid, the strongly adsorbed component and the weakly adsorbed component in the raw material solution are separated. On the other hand, in the washing mode, the eluent inlet,
Switching between the extract liquid outlet, the raw material solution inlet, and the raffinate liquid outlet and the circulation of the circulating liquid in the circulating fluid flow path are stopped (excluding the case where the circulating fluid flow path is washed). ).

The switching between the separation / purification mode and the washing mode can be manually performed by an operator. Further, after the simulated moving bed type separation apparatus is operated in the separation / refining mode for a certain period of time, the packed bed is washed by switching to the washing mode. The operation of switching the separation device to the separation / purification mode and operating may be repeated. Further, in the cleaning mode, a monitor for continuously measuring the concentration of the strongly adsorbed component and the weakly adsorbed component in the cleaning liquid extracted from the cleaning liquid discharge pipe is provided in the cleaning liquid discharge pipe. When it is detected that the concentration of the weakly adsorbed component is lower than the predetermined value, the simulated moving bed type separator may be automatically switched from the washing mode to the separation / purification mode again to continue the operation.

In the cleaning mode, the control device:
All the cleaning liquid injection pipes and the cleaning liquid discharge pipes may be opened at the same time, and control may be performed so that all the packed beds are cleaned at the same time. The on-off valve may be controlled so that several sets are opened and the packed bed is washed one by one or every several beds.

An eluent inlet and a raw material solution inlet are provided on the inlet side of each packed bed in the circulating fluid flow path, and an extract liquid outlet and a raffinate liquid outlet are connected to each packed bed in the circulating fluid flow path. In the washing mode, the eluent inlet and the raw material solution inlet are used as washing liquid injection means, and the extract liquid outlet and the raffinate are provided. A liquid outlet may be used as the washing liquid discharging means.

Examples of the washing liquid delivery means include various pumps, and specifically, any of positive displacement pumps such as a diaphragm pump and a plunger pump and turbo pumps such as a centrifugal pump can be used. Among these pumps, a diaphragm pump is most preferable because it can easily cope with high pressure and does not cause contamination of the cleaning liquid.

Other examples of the cleaning liquid delivery means include a cleaning liquid tank for extruding the cleaning liquid with a pressurized gas.

2. Embodiments of the Present Invention Hereinafter, embodiments of the simulated moving bed type separation apparatus of the present invention will be described.

FIG. 1 is a piping diagram schematically showing an example of a simulated moving bed type separation apparatus according to the present invention.

The simulated moving bed type separation apparatus shown in FIG. 1 comprises a column a, a column b, a column c,
And column d, and a pump P for circulating a circulating liquid through the columns a to d.

The columns a to d are filled with a separation filler.

The outlet side of the column a and the inlet side of the column b are connected by a pipe C _ab , the outlet side of the column b and the inlet side of the column c are connected by a pipe C _bc , and the outlet side of the column c and the column It is connected to the inlet side of d by a pipe _Ccd . The outlet side of the column d and the suction side of the pump P
Are connected by a pipe C _2, it is connected by a pipe C ₁ and the inlet side of the discharge side and the column a of the pump P. Therefore, the columns a to d, the pipe C ₁ , the pipe C ₂ , the pipe C _ab , the pipe C _bc , the pipe C _cd , and the pump P form a circulation channel FC as a whole. In the circulation channel FC, the circulating liquid flows in the direction indicated by the arrow in FIG.

In the portion near the inlet side of each of the columns a to d in the circulation flow channel FC, the raw material solution containing the component to be separated is supplied to the circulation flow channel FC through the raw material solution introduction lines F _a to F _a . and F _d, and desorbing liquid introducing line D _a to D _d is connected to supply an eluent to the circulation flow path FC.

On the other hand, the columns a to
d in the vicinity of each outlet side, the circulation channel F
And extract draw-out line E _a to E _d withdrawing the extract solution from C, raffinate draw-out line withdrawing raffinate from the circulation flow path FC R _a to R _d
And are connected.

The eluent introduction lines D _{a to} D _d and the raw material solution introduction lines F _{a to} F _d include an eluent supply line D for supplying an eluent to the eluent introduction lines D _{a to} D _d , It is connected to the raw material solution supply line F supplied to the feedstock introducing line F _a to F _d a. Eluent supply line D is connected to the eluent pump P _D at one end, the raw material solution supply line F is connected to the raw material solution pump P _F at one end.

On the downstream side of the eluent supply line D in the eluent introduction lines D _{a to} D _d , electromagnetic valves VD _{a to} V D
D _d is interposed, feedstock introducing line F _a to F electromagnetic on the downstream side of the raw material solution supply line F in _d valves V
F _{a to} VF _d are interposed.

On the other hand, the extract liquid extraction lines E _a to
The E _d, is interposed electromagnetic valve VE _a ~VE _d respectively, said extract draw-out line E _a to E extract attracted extract solution withdrawn from _d extract solution integrated draw-out line E When, it is connected to the extract draw pump P _E. The raffinate draw-out line R _a to R _d, each solenoid valve VR _a to VR _d
There is interposed, it said raffinate draw-out line R _a to R _d
Raffinate integration extracted attracted raffinate withdrawn from the extraction line R and the raffinate draw pump P _R are connected. The extract liquid integrated extraction line E is provided with a strongly adsorbed component concentration monitor EM, and the raffinate liquid integrated extraction line R is provided with a weakly adsorbed component concentration monitor RM. Incidentally, the extract draw pump P _E and raffinate draw pump P
_At least one of _R may be replaced with a pressure control valve. Further, only one of the strong adsorption component concentration monitor EM and the weak adsorption component concentration monitor RM may be attached.

[0060] These electromagnetic valves VF _a ~VF _d, solenoid valve VD _a ~VD _d, solenoid valves VE _a ~VE _d, solenoid valve VF _a ~VF _d, and the electromagnetic valve VR _a ~V
_Rd is opened and closed by a command from a control device (not shown). The controller is connected to a strongly adsorbed component concentration monitor EM provided on the extract liquid integrated extraction line E and a weakly adsorbed component concentration monitor RM provided on the raffinate liquid integrated extraction line R.

In the simulated moving bed type separation apparatus shown in FIG. 1, columns a to d correspond to a packed bed in the simulated moving bed type separation apparatus of the present invention, and the circulation channel FC is provided in the simulated moving bed type separation apparatus of the present invention. It corresponds to a circulating fluid flow path in the device. The eluent introduction lines D _{a to} D _d correspond to the eluent introduction ports in the simulated moving bed type separation apparatus of the present invention, and the extract liquid extraction lines E _{a to} E _d correspond to the simulated moving bed type separation apparatus of the present invention. This corresponds to the extract liquid outlet in the device. The feedstock introducing line F _a to F _d corresponds to feedstock introducing port in the simulated moving bed separation apparatus of the present invention, raffinate draw-out line R _a to R _d is simulated moving bed of the present invention This corresponds to a raffinate liquid outlet in the separation device. When the simulated moving bed type separation device is in the washing mode, the electromagnetic valves VD _{a to} VD _d function as cleaning liquid injection means in the simulated moving bed type separation device of the present invention, and the electromagnetic valves VE _a to VE _d.
The VE _d and solenoid valve VR _a ~VR _d, functions as washing liquid discharge means in the simulated moving bed separation apparatus of the present invention. The eluent pump P _D serves as a washing liquid supply means in the simulated moving bed separation apparatus of the present invention.

The operation of the simulated moving bed type separation apparatus shown in FIG. 1 will be described below.

In the simulated moving bed type separation apparatus, when the necessary components are separated and purified from the raw material solution containing a plurality of components, the eluent is introduced along the flow direction of the circulating liquid flowing through the circulation channel FC. one of the line D _a to D _d
One, one of the extract draw-out line E _a to E _d
One of the raw material solution introduction lines F _{a to} F _d and one of the raffinate solution extraction lines R _{a to} R _d include an eluent introduction line, an extract solution extraction line,
The electromagnetic valve VD _a is connected so as to communicate with the circulation channel FC in the order of the raw material solution introduction line and the raffinate liquid extraction line.
To VD _d , solenoid valve VE _{a to} VE _d , solenoid valve VF
_{a to} VF _d and the electromagnetic valves VR _{a to} VR _d are controlled by the control device.

More specifically, for example, the control device is configured to control the solenoid valve VD _a , the solenoid valve VE _a , the solenoid valve VF
_c, and the electromagnetic valve VR _c opened, by all the other electromagnetic valve closed, desorbing liquid introducing line D _a, extract draw lines E _a, feedstock introducing line F _c
And raffinate draw-out line R _c is circulating channel F
Communicate with C.

[0065] Thus, column a positioned between the desorbing liquid introducing line D _a and extract draw line E _a
Desorbing zone (IV) is formed, the concentration zone column b located between the extract draw-out line E _a and feedstock introducing line F _c (III) are formed. The feedstock introducing purified zone column c located between the line F _c and raffinate draw-out line R _c (II) is formed,
Raffinate draw-out line R _c and desorbing liquid introducing line D _a
The adsorption zone (I) is formed in the column d located between the two.

[0066] Therefore, in the column a desorption zone (IV) is formed, the eluent from the feedstock introducing line F _a is supplied to the circulation flow path FC, has been circulated in the circulation flow path FC, strongly adsorbable component The strongly adsorbed component adsorbed on the internal separation filler is desorbed by the circulating liquid containing neither the weakly adsorbed component nor the weakly adsorbed component, and moves into the circulating liquid. Therefore,
On the inlet side of the column a, the concentration of the strongly adsorbed component in the circulating liquid is close to 0, and the concentration of the strongly adsorbed component in the circulating liquid increases while proceeding through the column a. Out of the column a as a circulating liquid containing a large amount of Some of the circulating fluid flowing out of the column a is withdrawn from the extract draw-out line E _a as extract solution,
The remainder flows into column b.

In the column b in which the concentration zone (III) is formed, while the circulating liquid passes through the column b, the strongly adsorbed components in the circulating liquid are adsorbed by the packing material for separation. On the other hand, the weakly adsorbed components adsorbed on the column b move into the circulating liquid. Circulating liquid discharged from column b flows into the column c with raw material solution supplied from feedstock introducing line F _c.

In the column c in which the purification zone (II) is formed, the strongly adsorbed components contained in the raw material solution and the circulating liquid are adsorbed by the adsorbent for separation, and the weakly adsorbed components adsorbed by the adsorbent for separation are adsorbed. Migrates to the circulating fluid. From the outlet of the column c, a circulating liquid containing a large amount of weakly adsorbed components flows out. Part of the circulating liquid discharged from column c is withdrawn from the raffinate draw-out line R _c to the outside as raffinate, the remainder of the circulating fluid flows into the column d.

In the column d in which the adsorption zone (I) has been formed, the weakly adsorbed components contained in the circulating liquid at a high concentration are adsorbed by the separation packing material, and the weakly adsorbed components and The circulating liquid from the column d, from which the circulating liquid containing no strongly adsorbed component flows, flows through the pipe C ₂ , the pump P, and the pipe C ₁ again into the column a.

After a lapse of a predetermined time, the control device determines whether the solenoid valve VD _a , the solenoid valve VE _a , the solenoid valve VF _c ,
And an electromagnetic valve VR _c is closed, instead, the electromagnetic valve VD _b, the electromagnetic valve VE _b, the electromagnetic valve VE _d, and the electromagnetic valve VR _d outputs a command to the effect that the opening, the desorbing liquid introducing line D _a switch to desorbing liquid introducing line D _b,
Switch the extract draw-out line E _a to extract draw line E _b, switching the feedstock introducing line F _c to feedstock introducing line E _d, raffinate draw-out line R _c the raffinate draw-out line R Switch to _d . By this switching, the desorption zone (IV) moves from column a to column b, the concentration zone (III) moves from column b to column c, and the purification zone (II) moves from column c to column d. Then, the adsorption zone (I) moves from the column d to the column a.

Accordingly, in the column b, the strongly adsorbed component adsorbed on the separation filler is desorbed by the eluent supplied from the eluent supply line D. A part of the circulating liquid flowing out of the column b is extracted as an extract liquid from the extract liquid extraction line _Eb , and the rest flows into the column c.

In the column c, the strongly adsorbed component in the circulating liquid is adsorbed by the separation packing material, and the weakly adsorbed component adsorbed on the column c is transferred into the circulating liquid, and passes through the column c. Meanwhile, the concentration of the strongly adsorbed component in the circulating liquid decreases, and the concentration of the weakly adsorbed component increases.

[0073] circulating liquid discharged from column c, the column d with raw material solution supplied from feedstock introducing line E _d
Flows into. In the column d, the strongly adsorbed components contained in the raw material solution and the circulating liquid are adsorbed by the separating adsorbent, and the weakly adsorbed components adsorbed by the separating adsorbent are transferred to the circulating liquid. Part of the circulating liquid discharged from column d is withdrawn from the raffinate draw-out line R _d to the outside as raffinate, the remainder of the circulating fluid flows into the column a.

Then, in column a, the weakly adsorbed component and the strongly adsorbed component in the circulating liquid are adsorbed, and from column a, the circulating liquid containing no weakly adsorbed component and strongly adsorbed component flows out of column a. The circulating liquid that has flowed out is again in column b
Flows into.

After a further elapse of a predetermined time, the control device closes the solenoid valves VD _b , VE _b , VE _d , and VR _d , and instead,
Solenoid valve VD _c , solenoid valve VE _c , solenoid valve VF
_a, and the electromagnetic valve VR _a outputs an instruction to open, switching the desorbing liquid introducing line D _b in desorbing liquid introducing line D _c, extract draw line E _b the extract draw-out line E switch to _c, switching the feedstock introducing line E _d to feedstock introducing line F _a, raffinate draw-out line R _d the raffinate draw-out line R _a
Switch to Thereby, the desorption zone (IV) moves from column b to column c, the concentration zone (III) moves from column c to column d, and the purification zone (II) moves to column d.
From the column a, and the adsorption zone (I)
To column b.

In the separation / purification mode, as described above, the solenoid valves VF _{a to} VF _d and the solenoid valves VD _a
To VD _d , solenoid valve VE _{a to} VE _d , solenoid valve VF
_{a to} VF _d , and electromagnetic valves VR _{a to} VR _d , eluent introduction lines D _{a to} D _d , extract liquid extraction lines E _{a to} E _d , raw material solution introduction lines F _{a to} F _d ,
And by switching the raffinate draw-out line R _a to R _d, desorbing zone (IV) and the concentration zone (III) and the purified zone (II) and the adsorption zone (I), but the column a~d
Move up.

In the cleaning mode, the pumps P and P
Stop _F. And electromagnetic valves VD _{a to} VD _d ,
Electromagnetic valve VE _a ~VE _d or electromagnetic valve VR _a ~V
All the R _d is opened, to start the eluent pump P _D.

The eluent supplied from the eluent pump P _D passes through the eluent introduction lines D _{a to} D _d and passes through the column a.
~ D. Then, the strongly adsorbed components, weakly adsorbed components, impurities, etc. remaining in the columns a to d are removed from the columns a to d.
The eluent was extracted from the extract draw-out line E _a to E _d or raffinate draw-out line R _a to R
Exhausted through _d .

Further, the flow resistance of the cleaning liquid differs for each packed bed, and if the cleaning liquid is distributed to all the packed beds at the same time,
The washing liquid may hardly flow through the packed bed having a large flow resistance. In such a case, cleaning can be performed by supplying a cleaning liquid to each packed bed.

For example, when washing column a,
First, it stops the pump P and P _F. Then, the electromagnetic valve VD _a, opens the electromagnetic valve VE _a or VR _a, the other electromagnetic valve is closed. The pump P _D Start, the cleaning liquid is supplied to the column a through eluant supply line D and desorbing liquid introducing line D _a, extract draw line E _a or raffinate draw-out line R _a
Extract from

The concentration monitor EM for strongly adsorbed components provided in the extract liquid integrated extraction line E or the weakly adsorbed component concentration monitor E provided in the raffinate liquid integrated extraction line R
In R, when the concentration of the strongly adsorbed component or the weakly adsorbed component in the cleaning liquid is equal to or lower than a predetermined value, it can be determined that the cleaning of the column a has been completed.

Similarly, when washing column b,
The pump P and P _F in a state of stopping the electromagnetic valve V
D _b and opens the electromagnetic valve VE _b or VR _b, to start the eluent pump P _D the other electromagnetic valve is closed, the washing solution, eluent supply line D and desorbing liquid introducing line D _b
To the column b, and is extracted from the extract liquid extraction line _Eb or the raffinate liquid extraction line _Rb .

The columns c and d can be similarly washed.

[0084] Further, in the above simulated moving bed separation apparatus, to replace the raw material solution in the raw material solution tank, not shown in the cleaning liquid, try to wash the washing liquid by raw solution pump P _F instead of the eluent pump P _D It may be fed to the column with, also, the eluent pump P _D connected to the raw material solution supply line F by the three-way valve TV, and start the eluent pump P _D in this state, through the raw material solution supply line F It may be supplied to the column to be washed.

Either the strongly adsorbed component concentration monitor EM provided in the extract liquid integrated extraction line E or the weakly adsorbed component concentration monitor RM provided in the raffinate liquid integrated extraction line R is either strongly adsorbed or weakly adsorbed. Upon detecting that the concentration of the adsorbed component is lower than the specified value, the simulated moving bed type separator of FIG. 1 is automatically switched from the washing mode to the separation / purification mode.

FIG. 2 shows a simulated moving bed type separation apparatus of FIG. 1 in which a rotary valve is used to switch among a raw material solution introduction line, an eluent introduction line, an extract solution extraction line, and a raffinate solution extraction line. It is a piping diagram showing an outline of an example of a bed type separation device.

In the simulated moving bed type separation apparatus shown in FIG.
As in the simulated moving bed type separation apparatus of FIG. 1, eluent introduction lines D _{a to} D _d and raw material solution introduction lines F _{a to} F _d are connected to the inlet side of columns _a to _d in the circulation channel FC, respectively. is, on the outlet side of the column a~d in the circulation flow path FC, respectively extract draw line E _a to E _d and raffinate draw line R _a to R _d are connected. The extract liquid extraction line E is provided with a strong adsorption component concentration monitor EM, and the raffinate liquid extraction line R is provided with a weak adsorption component concentration monitor RM.

The eluent introduction lines D _{a to} D _d are connected to an eluent supply line D via a rotary valve RV _D , and the raw material introduction lines F _{a to} F _d are supplied via a rotary valve RV _F It is connected to the solution supply line F. The eluent supply line D and the raw material solution supply line F, as with simulated moving bed separation apparatus of FIG. 1, are respectively connected to the eluent pump P _D and the raw material solution pump P _F. The rotary valve RV _D is connected to the eluent introduction line _Da.
~D Select one of the _d communicates with the eluent supply line D, and has a function of other desorbing liquid introducing line D _a ~D _d and a closed state. Rotary valve RV _F is,
Feedstock introducing line F _a to F by selecting one of the _d communicates with the raw material solution supply line F, and has a function of the other feedstock introducing line F _a to F _d and closed. Rotary valve RV in the eluent supply line D
Between the _D and eluent pump P _D, three-way switching valve TV
The three-way switching valve TV is connected to a raw material solution supply line F.

The raffinate liquid extraction lines R _{a to} R _d are:
Through the rotary valve RV _R, are connected to the raffinate integrated draw-out line R, extract draw line E _a to E _d via the rotary valve RV _E, connected to the extract solution integrated draw-out line E Have been. Rotary valve RV _R are raffinate draw-out line R _a
Select one of the to R _d in communication with the raffinate integrated draw-out line R, other raffinate draw-out line R
It has the function of a closed state _a to R _d. Rotary valve RV _E is extract draw lines E _a ~
One of E _d is selected and communicated with the extract liquid integrated extraction line E, and the other extract liquid extraction lines E _{a to} E _d are closed. In addition,
The rotary valve RV _D, RV _E, switching the RV _F, and RV _R are controlled by a not shown control device.

In the simulated moving bed type separation apparatus of FIG. 2, columns a to d correspond to the packed beds in the simulated moving bed type separation apparatus of the present invention, and the circulation channel FC is provided by the simulated moving bed type separation apparatus of the present invention. It corresponds to a circulating fluid flow path in the device. The eluent introduction lines D _{a to} D _d correspond to the eluent introduction ports in the simulated moving bed type separation device of the present invention, and the extract extraction lines E _{a to} E _d correspond to the simulated moving bed separation device of the present invention. Corresponds to the extract liquid outlet. The raw material solution introduction lines F _{a to} F _d correspond to the raw material solution introduction ports in the simulated moving bed type separation device of the present invention, and the raffinate extraction lines _{Ra to} R _d correspond to the simulated moving bed type separation device of the present invention. This corresponds to a raffinate liquid outlet. Incidentally, the eluent supply line D, a eluent pump P _D, solenoid valves VD _a ~
And VD _d, and the electromagnetic valve VE _a ~VE _d, electromagnetic valve V
And F _a ~VF _d, and the electromagnetic valve VR _a ~VR _d, rotary valve RV _D, RV _E, and RV _F, and RV _R, and the three-way switching valve TV, simulated moving bed separation apparatus of FIG. 2 is washed When in the mode, it functions as a packed bed washing means in the simulated moving bed type separation apparatus of the present invention. In this case, the eluent supply line D, a eluent pump P _D, a solenoid valve VD _a to VD _d, solenoid valve VF _a ~VF _d
When the rotary valve RV _D and RV _F, and the three-way switching valve TV, functions as washing liquid filling means in the simulated moving bed separation apparatus of the present invention, the electromagnetic valve VE _a ~VE _d
An electromagnetic valve VR _a to VR _d and a rotary valve RV
The _E and RV _R, which functions as a cleaning liquid discharging means in the simulated moving bed separation apparatus of the present invention. The eluent pump P _D functions as washing liquid sending means in the simulated moving bed separation apparatus of the present invention.

The operation of the simulated moving bed type separation apparatus shown in FIG. 2 will be described below.

In the separation / purification mode, the circulation channel F
The eluent is connected to the circulation channel FC in the order of the eluent introduction line, the extract liquid extraction line, the raw material solution introduction line, and the raffinate liquid extraction line along the flow direction of the circulating liquid flowing through C. one of the introduction line D _a to D _d
One of the extract extraction lines E _{a to} E _d
One of the raw material solution introduction lines F _{a to} F _d and one of the raffinate extraction lines R _{a to} R _d
Rotary valve RV _D respectively, RV _F, RV _E, and the RV _R, eluent supply line D, the raw material solution supply line F, extract integrated extraction line E, and raffinate integrated extraction line to R in communication with.

[0093] For example, in the example shown in FIG. 2, the desorbing liquid introducing line D _a and feedstock introducing line F is, by the rotary valve RV _D and the rotary valve RV _F, respectively eluent supply line D and the raw material solution communicating with the supply line F, desorbing liquid introducing line D _b to D _d and feedstock introducing line F _a, becomes closed and F _b, and E _d. The extract draw-out line E _a and the raffinate draw-out line R _c is, rotary valve RV _E
And by the rotary valve RV _R, respectively communicating with the extract integrated extraction line E and raffinate integrated draw-out lines R, extract draw line E _b to E
d and raffinate withdrawal lines R _a , R _b , and R _d
Is closed.

Therefore, in the column a between the eluent introduction line D _a and the extract extraction line E _a , a desorption zone (IV) for desorbing strongly adsorbed components is formed,
In column b lies between the extract draw-out line E _a to feedstock introducing line F _c, are formed strong enrichment zone which adsorbate is desorbed adsorbed weakly adsorbed component (III) is, feedstock introducing line F in column c is between up raffinate draw-out line R _c from _c, purified zone strongly adsorbed components in the raw material solution is separated from the weakly adsorbed component is adsorbed (II) is formed, raffinate draw-out line in is between from R _c to desorbing liquid introducing line D _a column d, adsorption zones weakly adsorbed components in the circulating fluid is adsorbed (I) is formed.

[0095] When the predetermined time has elapsed, the controller outputs a command for switching the rotary valve _{RV D, RV E, RV F} , and the RV _R.

By this switching, the eluent introduction line D _a
Is switched to desorbing liquid introducing line D _b, extract draw line E _a is extract draw line E _b
Switched to, feedstock introducing line F _c is switched to feedstock introducing line E _d, raffinate draw-out line R _c is switched to the raffinate draw-out line R _d. Therefore, a desorption zone (IV) is formed in column b, a concentration zone (III) is formed in column c, and a column d is formed.
A purification zone (II) is formed in column
(I) is formed.

As described above, the rotary valves RV _D , R
V _E, RV _F, and the RV _R, desorbing liquid introducing line D _a to D _d and, extract draw-out lines E _a to E _d
And the raw material solution introduction lines F _{a to} F _d and the raffinate extraction lines R _{a to} R _d are sequentially switched to form a desorption zone (IV), a concentration zone (III), and a purification zone (I
I) and the adsorption zone (I) move on columns ad.

FIG. 3 shows a state where the simulated moving bed type separation apparatus of FIG. 2 is switched to the washing mode.

[0099] As shown in FIG. 3, when the simulated moving bed separation apparatus is switched to the cleaning mode, the pump P and the pump P _F stops, it stops the flow of circulating fluid flowing through the circulation flow path F .

[0100] In this state, for example when attempting to wash the column a, eluent supply line D is communicated with the desorbing liquid introducing line D _a, or three-way switching valve TV eluent supply line D switches the raw material Solution introduction line _Fa
So as to communicate with the switches and the rotary valve RV _D and RV _F, extract solution integrated draw-out line E communicates with the extract draw-out line R _a, raffinate integrated draw-out line R is raffinate draw so as to communicate with the line R _a, switching between the rotary valve RV _E and RV _R.

[0102] In this state, when you start the eluent pump P _D, eluent stock solution eluent supply line D and desorbing liquid introducing line D _a or from the eluent supply line D, via the three-way switching valve TV through inlet line F _a and flows into the column a. Eluent which has flowed into the column a passes through the extract draw-out line E _a or raffinate draw-out line R _a, extract solution integrated draw-out line E
Alternatively, it is discharged to the outside from the raffinate liquid integrated extraction line R.

When the concentration of the strongly adsorbed component detected by the strongly adsorbed component concentration monitor EM and the concentration of the weakly adsorbed component detected by the weakly adsorbed component concentration monitor RM become lower than a predetermined value,
The control device determines that the cleaning of the column a has been completed,
By switching between the rotary valve RV _D and RV _F, communicating the eluent supply line D is communicated with the desorbing liquid introducing line D _b, or the eluent supply line D switches the three-way switching valve TV to the feedstock introducing line F _b Let it. And by switching between the rotary valve RV _E and RV _R, communicates the extract solution integrated extraction line E to extract draw line E _b, the raffinate integrated draw-out line R in raffinate draw-out line R _b Communicate. And
Start eluent pump P _D is circulated eluent to the column b in this state to wash the column b. At the time of washing, either the strongly-adsorbed component concentration monitor E provided on the extract liquid integrated extraction line E or the weakly-adsorbed component concentration monitor R provided on the raffinate liquid integrated extraction line R is used for the strong adsorbed component monitor. Alternatively, when detecting that the concentration of the weakly adsorbed component is lower than the specified value, the control device determines that the washing of the column b has been completed. Hereinafter, the same can be sequentially performed for the columns c and d.

[0103]

According to the present invention, there is provided a simulated moving bed type separation apparatus capable of cleaning a circulation fluid flow path in a short time. Specifically, there is provided a simulated moving bed type separation apparatus that can simultaneously wash all the packed beds provided in the circulating fluid flow path or wash only the packed beds that need to be washed.

In the simulated moving bed type separation apparatus provided by the present invention, when a plurality of packed beds are washed,
Since the packed bed is connected in parallel to flow a washing solution such as an eluent, the pressure loss during washing is extremely small. Therefore, the cleaning solution can be flown at a high flow rate through the packed bed and the circulating fluid flow path, and thus the packed bed and the circulating fluid flow path can be cleaned in a short time. In addition, the problem that impurities accumulated in one packed bed are circulated in the circulating fluid channel by the cleaning liquid flowing in the circulating fluid channel and contaminate the other packed beds is also solved.

In the simulated moving bed type separation apparatus provided by the present invention, an eluent inlet and a raw material solution inlet are provided near the inlet of each packed bed, and the extract liquid is provided near the outlet of each packed bed. When the packed bed is washed, a washing liquid is injected from the eluate inlet and the raw material solution inlet, and the washing liquid is injected through the extract liquid outlet and the raffinate liquid outlet. The simulated moving bed type separation apparatus of the aspect of discharging the wastewater has a feature that the raw material solution inlet, the extract liquid outlet and the raffinate outlet can be washed simultaneously with the packed bed.

[Brief description of the drawings]

FIG. 1 is a piping diagram showing one embodiment of a simulated moving bed type separation apparatus of the present invention.

FIG. 2 is a simulated moving bed type separation apparatus of FIG. 1 in which a rotary valve switches between a raw material solution introduction line, an eluent introduction line, an extract solution extraction line, and a raffinate solution extraction line. It is a piping diagram which shows the outline of an example of a moving bed type separation apparatus.

FIG. 3 is a piping diagram showing a state in which a column is washed in the simulated moving bed type separation apparatus of FIG. 2;

[Explanation of symbols]

ad: columns, C _ab , C _cd , C _cd , C ₁ , C _2.
..Piping, FC: circulation channel, D _{a to} D _d: eluent introduction line, E _{a to} E _d: extract liquid extraction line, F _{a to} F _d: raw material solution Introduction line, _Ra ~
R _d: raffinate liquid extraction line, D: eluent supply line, E: extract liquid integrated extraction line, F: raw material supply line, R: raffinate liquid integrated extraction Line, P _D ··· Eluent pump, P _F ·
· Raw material solution pump, PE · · · extract draw pump, P _R · · · raffinate draw pump, RV
_{D, RV F, RV E,} RV R ··· rotary valve,
_{VD a ~VD d, VE a ~VE} d, VF a ~VF d, V
_{Ra to} VR _d: Electromagnetic valve, TV: Three-way switching valve, EM: Strongly adsorbed component concentration monitor, RM: Weakly adsorbed component concentration monitor

────────────────────────────────────────────────── ───

[Procedure amendment]

[Submission date] January 7, 1998

[Procedure amendment 1]

[Document name to be amended] Drawing

[Correction target item name] All figures

[Correction method] Change

[Correction contents]

FIG.

FIG. 2

FIG. 3

Claims (2)

[Claims] 1. A circulating fluid flow path having two or more packed beds filled with a separating filler therein and connected in series and endlessly, and forcibly circulating a liquid therein. An eluent inlet for introducing an eluent into the circulating fluid channel, and an extract liquid outlet for extracting a solution containing a large amount of strongly adsorbed components in the raw material solution containing the component to be separated from the circulating fluid channel, A source solution inlet for introducing the source solution into the circulating fluid channel, a raffinate liquid outlet for extracting a solution containing a large amount of weakly adsorbed components in the source solution from the circulating fluid channel, and the eluent The inlet, the extract liquid outlet, the raw material solution inlet, and the raffinate liquid outlet are arranged along the circulation direction of the liquid circulating in the circulating fluid flow path, the eluent inlet, the extract liquid outlet, the raw material solution. Inlet, raffy Are arranged in the order of the outlet
And in the pseudo moving bed type separation device provided so as to intermittently move on the circulating fluid flow path while maintaining the order, the inside of the packed bed from one end of each packed bed. A simulated moving bed type separation apparatus comprising a packed bed washing means for introducing a washing liquid to be washed and washing the packed bed. 2. The packed bed cleaning means according to claim 1, wherein one or more columns are used as one unit, and a cleaning liquid is supplied for each unit, and a unit for supplying the cleaning liquid is switched at regular intervals. The simulated moving bed type separation apparatus according to claim 1, which is a bed washing means.