CN106166402B - A kind of moving bed imitation chromatogram separation facility - Google Patents
A kind of moving bed imitation chromatogram separation facility Download PDFInfo
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- CN106166402B CN106166402B CN201610832972.6A CN201610832972A CN106166402B CN 106166402 B CN106166402 B CN 106166402B CN 201610832972 A CN201610832972 A CN 201610832972A CN 106166402 B CN106166402 B CN 106166402B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
- B01D15/10—Selective adsorption, e.g. chromatography characterised by constructional or operational features
- B01D15/18—Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to flow patterns
- B01D15/1892—Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to flow patterns the sorbent material moving as a whole, e.g. continuous annular chromatography, true moving beds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
- B01D15/10—Selective adsorption, e.g. chromatography characterised by constructional or operational features
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
- B01D15/10—Selective adsorption, e.g. chromatography characterised by constructional or operational features
- B01D15/18—Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to flow patterns
- B01D15/1864—Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to flow patterns using two or more columns
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- Treatment Of Liquids With Adsorbents In General (AREA)
Abstract
It is an object of the invention to be directed to the problems such as existing SMB equipment operating modes are relatively fixed, a kind of moving bed imitation chromatogram separation facility is provided, belongs to technical field of chromatography separation.The device is made of 8~30 root chromatogram columns, per root chromatogram column 6 intake lines, 4 output pipes and 1 circulation line are controlled by 11 two-port valves, all respective working conditions of two-port valve are controlled by PLC or single-chip computer control system, a variety of operating modes can be set, including：Setting participates in the chromatographic column number of separation, sets multi-zone, setting interception pipeline, and setting area interband is continuous or independent operating process, and setting either synchronously or asynchronously switch mode, the device pipeline is easy to connect, and operation is flexible, easily safeguards, can complete multicomponent separation.
Description
Technical field
The invention belongs to technical field of chromatography separation, more particularly to a kind of general-purpose simulation mobile bed chromatic separator.
Background technology
Simulated Moving Bed Chromatography (abbreviation SMB) technology have high separation, high yield, in high yield, high efficiency and company
Continuous automatic running scheme, is high-end separation means.Simulated movable bed chromatography device is connected into circulation loop by several tail prime ministers
Chromatographic column forms, by regularly moving mobile phase import with the position of efflux outlet along the flow direction of mobile phase come mould
The move counter-current for intending stationary phase and mobile phase flows, and then realizes the separation of different component.SMB operating modes include setting and participate in
The chromatographic column number of separation divides different function area, each area's chromatographic column of setting, and Simulated Moving Bed Chromatography separation principle determines work
The diversity of operation mode；And operating mode is the key factor that the separation of Optimized Simulated mobile bed chromatic is examined or check first, but practical
On SMB equipment mostly restricted by switching valve and its software kit using relatively fixed operational mode, same SMB equipment
It is difficult to realize the conversion between a variety of different modes.
Invention content
The present invention provides a kind of general-purpose simulation mobile bed chromatic separator.The device is each chromatography in SMB systems
Column arranges 11 two-port valves, can set a variety of operating modes, realizes multicomponent separation.
A kind of Simulation moving bed device, including M root chromatogram columns, 4≤M≤30 connect respectively per root chromatogram column entrance and exit
Access port is mostly logical and outlet is mostly logical, and the more reduction of fractions to a common denominators of entrance do not connect the circulation line of 6 intake lines and previous root chromatogram column, go out
The more reduction of fractions to a common denominators of mouth do not connect 4 output pipes and the circulation line of current chromatographic column；The every intake line or efferent duct
Road connects respectively with corresponding input bus or output bus；Material liquid, eluent are respectively by corresponding input bus the input phase
Answer the intake line of chromatographic column；It is more that the circulation line connects the previous more logical and current chromatography column inlets in root chromatogram column outlet
It is logical, all chromatographic columns is made to pass through circulation line tail head and are connected；Various column effluents in addition to efflux is recycled respectively by
Corresponding chromatographic column is output to corresponding output bus by corresponding output pipe；
Material liquid, eluent are stored in corresponding fluid reservoir；From output bus flow out various column effluents be
The system efflux of Simulation moving bed is stored in corresponding fluid reservoir；
Two-port valve is respectively provided on intake line, output pipe and circulation line per root chromatogram column；The two-port valve is by electricity
Magnet valve and check (non-return) valve composition, and each two-port valve is controlled to be turned on and off state by PLC or single-chip computer control system；
The chromatographic column works under the constant temperature in the range of -10 DEG C~200 DEG C；
Above-mentioned Simulation moving bed device, can set multi-zone SMB：Such as three band a-b-c, four band SMB：A-b-c-d, five
Band SMB：For six bands of a-b-c-d-e to more bands, a, b, c, d, e refer to every band chromatographic column number, and open loop can be set to input material liquid
Or the pattern of eluent pattern, adsorption zone and the fine Disengagement zone of slow component are continuous, the pattern of elution zone independence, each area's independence work
The sequence SMB operational modes of work.
Further, the chromatographic column number that SMB participates in separation may be selected, i.e., in above-mentioned Simulation moving bed device：Described
The chromatographic column of separation process is participated in device as N roots, 3≤N≤M；N root chromatogram columns are connected by circulation line tail head, are formed back
Road.
Further, an output bus is connect by above-mentioned Simulation moving bed device with an input bus, is formed and is cut
Take pipeline.
Further, above-mentioned Simulation moving bed device, can realize interception part efflux and continuous backflow refines, and beat
Open the output pipe two-port valve being connected with the interception pipeline of the chromatographic column of current output efflux and latter color of the column
Spectrum column with the intake line two-port valve that is connected of interception pipeline, form return line, and set on return line defeated
Send pump；
Or 1 threeway and 1 delivery pump are set in pipeline is intercepted, a mouth of the threeway flows out for exporting
Liquid opens simultaneously the output pipe two-port valve being connected with the interception pipeline and the column of the chromatographic column of current output efflux
The intake line two-port valve being connected with the interception pipeline of latter root chromatogram column, equally constitutes return line；
Also, above two is formed in the mode of return line, will be current when the return line of current chromatographic column is opened
Chromatographic column circulation line is closed.
Alternatively, above-mentioned Simulation moving bed device, can realize interception part efflux and feed back to sample introduction entrance or wash
De- liquid entrance opens the output pipe two-port valve being connected with the interception pipeline of the chromatographic column of current output efflux and except this
Except the latter root chromatogram column of column any one root chromatogram column with the intake line two-port valve that is connected of interception pipeline, form around
Cross pipeline；
Described bypass sets 0~1 delivery pump in pipeline.
Further, above-mentioned Simulation moving bed device, can set either synchronously or asynchronously switch mode, for same work
Operation mode in switching cycle, sets import, outlet port by control system time segment, adjusts each functional areas band
Length, that is, each band chromatographic column number.
Further, above-mentioned Simulation moving bed device, the serial number that the M root chromatogram columns are arranged in order：Z1、Z2、
Z3, Z4, Z5 ..., Z (n-1), Zn, Z (n+1) ..., ZM, then in the N root chromatogram columns, come the adjacent chromatographic column at both ends
Tail head is connected, and other chromatographic column tail head separately are connected, and chromatographic column tail head is connected as the circulation line, all circulation pipes
Road is isometric；
When N is even number, the connection mode of N root chromatogram columns is：Z1、Z3、Z5、…、Z(N-3)、Z(N-1)、ZN、Z(N-2)、Z
(N-4) ..., Z4, Z2, Z1, i.e.,：By the increased direction of odd number, odd number chromatographic column tail prime minister is connected to one end Z (N-1), Z (N-1) with
ZN tails head is connected, and then, reduces direction by even number, even number chromatographic column tail prime minister is connected to other end Z2, Z2 and Z1 tail head and is connected, structure
Into the circuit of N root chromatogram columns, it is connected for " fried dough twist formula " tail head；
When N is odd number, the connection mode of N root chromatogram columns is：Z1、Z3、Z5、…、Z(N-4)、Z(N-2)、ZN、Z(N-1)、Z
(N-3) ..., Z4, Z2, Z1, i.e.,：By the increased direction of odd number, odd number chromatographic column tail prime minister is connected to one end ZN, ZN and Z (N-1) tail
Head is connected, and then, reduces direction by even number, even number chromatographic column tail prime minister is connected to other end Z2, Z2 and Z1 tail head and is connected, and forms N
The circuit of root chromatogram column is connected for " fried dough twist formula " tail head；
The connecting pipeline in a manner that " fried dough twist formula " tail head is connected, can make the liquid recycled of circulation line have approximation
Transmission process, avoid differential diffusion.
Further, above-mentioned Simulation moving bed device, the arrangement mode of the M root chromatogram columns is word order, annular
When modes, " fried dough twist formula " tail head is connected conveniently, and pipeloop is isometric for arrangement or rectangular arranged.
Further, above-mentioned Simulation moving bed device, can set multiple-working mode to work at the same time, by N root chromatogram columns
Simulation moving bed be decomposed into 2 sets of Simulation moving bed systems, i.e.,：L root chromatogram column tails head is connected to form a set of Simulation moving bed, and 3
≤ L≤(N-3), residue (N-L) root chromatogram column tail head are connected to form other set Simulation moving bed, 2 sets of Simulation moving bed systems
For independent operation mode, parallel running mode or series operation pattern.
Further, above-mentioned Simulation moving bed device disconnects the connecting pipeline between 2 sets of Simulation moving beds, being capable of structure
Different Simulation moving bed systems are covered into number, number set Simulation moving bed system is independent operation mode, parallel running mode or string
Join operational mode.
Further, all chromatographic columns are set to a region by above-mentioned Simulation moving bed device, and all two-port valves are set
Another region is placed in, temperature control is carried out to chromatography columnar region.
Further, above-mentioned Simulation moving bed device is equipped with filter, on-line degassing machine, circulation pipe on input bus
Road is equipped with flowmeter, and the detector of flowmeter, solution concentration and purity is equipped on output bus.
Further, above-mentioned Simulation moving bed device, with pipeline that operating mode is unrelated can corresponding how logical or
It is sealed at threeway with plug, to extend the related two-port valve service life.
Compared with prior art, advantage of the invention is that：
1st, the present apparatus has multiple functions：SMB is set to participate in the chromatographic column number of separation；Multi-zone SMB is set：Such as three bands
A-b-c, four band SMB：A-b-c-d, five band SMB：A-b-c-d-e, for six bands to more bands, a, b, c, d refer to every band chromatographic column number；
Setting area interband continuous operation or independent operation mode；Open loop sample introduction and the pattern of sampling are set；Setting either synchronously or asynchronously switches
Pattern；Interception part efflux simultaneously feeds back to sample introduction entrance or eluent entrance；Multiple-working mode works at the same time；It completes multigroup
Separation etc..
2nd, two-port valve operation is flexible, easily safeguards.
3rd, pipeline is easy to connect.
4th, valve and chromatographic column subregion are placed, can be to chromatographic column entirety temperature control.
Description of the drawings
Fig. 1 is a kind of Simulation moving bed schematic device of 8 root chromatogram column, which is a circuit, eight
Zone, 1-1-1-1-1-1-1-1, the strong absorbed component A of three components of separation, intermediate adsorption component B and weakly adsorbed components C.
Fig. 2 is a kind of Simulation moving bed schematic device of 8 root chromatogram column, which is a circuit, six
Zone, 1-1-2-1-1-2 detach three component A, B and C.It can be at corresponding more logical or threeways with the pipeline that operating mode is unrelated
It is sealed with plug.
Fig. 3 is a kind of Simulation moving bed schematic device of 8 root chromatogram column, which is a circuit, four
Zone, 2-2-2-2 detach two components A, B.
Fig. 4 is a kind of Simulation moving bed schematic device of 8 root chromatogram column, which is a circuit, six
Zone, wherein 1-1-2-1-1-2, first band independence and gradient elution detach three component A, B and C.
Fig. 5 is a kind of Simulation moving bed schematic device of 8 root chromatogram column, execution sequence chromatographic isolation, 4 root chromatogram columns ginseng
With detaching, each band independent operating or four sections of fraction As, B, C and W of separation or gradient elution is used.
Fig. 6 is a kind of Simulation moving bed schematic device of 8 root chromatogram column, which is " fried dough twist formula " tail prime minister
Even.
Fig. 7 is a kind of Simulation moving bed schematic device of 8 root chromatogram column, which is " fried dough twist formula " tail prime minister
Even, two 1-1-2 Simulation moving beds circuits, separation component A, B and C.
Wherein, Zn：N-th root chromatogram column, n：Chromatographic column serial number, Lmi：Input or output bus, m=1 represent input, m=2
Represent output, i for input or output bus serial number, Lnmi：N-th root chromatogram column input/output pipeline；Vnmi：The two-way of Lnmi
Valve, Tn：Circulation line two-port valve；
F：Material liquid fluid reservoir, D or Dq：Eluent D or eluent Dq fluid reservoirs, q：Eluent serial number, A：Separation component A
Fluid reservoir, B：Component B fluid reservoirs, C：Component C fluid reservoirs, W：Component W fluid reservoirs, Pi：The delivery pump of i-th input bus.
Specific embodiment
Using 8 root chromatogram column Simulation moving bed devices, as embodiment, the present invention is described in further detail below.
Embodiment 1
A kind of Simulation moving bed device, including 8 identical chromatographic columns, the n-th root chromatogram column Zn entrance and exits connect respectively
Access port is mostly logical and outlet is mostly logical, and the more reduction of fractions to a common denominators of entrance do not connect the circulation line T (n- of 6 intake lines and previous root chromatogram column
1) more reduction of fractions to a common denominators, are exported and do not connect 4 output pipes and the circulation line Tn of current chromatographic column, totally 11 pipelines；Material liquid, elution
Liquid is pumped into respective intake line by corresponding delivery pump via input bus respectively；Circulation line connects previous root chromatogram column Z
(n-1) outlet and current chromatographic column Zn entrances, make all chromatographic column tail head be connected；Various chromatographic columns in addition to efflux is recycled
Efflux imports corresponding output bus via respective output pipe respectively；Material liquid, eluent are stored in corresponding liquid storage
In tank；The system efflux of the solution, that is, Simulation moving bed flowed out from output bus is stored in corresponding fluid reservoir；Chromatographic column
All intake lines, all output pipes and all circulation lines be respectively provided with two-port valve；Chromatographic column works at room temperature；Two-way
Valve is made of solenoid valve and check (non-return) valve, is controlled the respective working condition of all two-port valves by PLC or single-chip computer control system or is opened
Or it closes.Carrying out practically step is embodied by the open and close state of each two-port valve, here, only describing the opening state of chromatographic column, is closed
Closed state does not repeat, and the Tn that chromatographic column circulation line two-port valve is only set with export direction is represented.
Simulation moving bed device shown in FIG. 1 is specially：If there are one circuit, eight zone, 1-1-1-1-1-1-1-1,
Three components are detached, respectively strong absorbed component A, intermediate adsorption component B and weakly adsorbed components C；
In the apparatus, material liquid is pumped into input bus L11 in fluid reservoir F by infusion pump P1, and eluent is in fluid reservoir D
In input bus L12 is pumped by infusion pump P2, component A enters fluid reservoir A through output bus L24 after separation, and component B is total through exporting
Line L23 enters fluid reservoir B, and component C enters fluid reservoir C through output bus L22；
An output bus therein and an input bus therein are connected, forms interception pipeline, L24-L16, L23-
L15、L22-L14、L21-L13；
One threeway and a mobile phase delivery pump P6, the mouth output of threeway are set in pipeline L24-L16 is intercepted
The system efflux A of the interception pipeline opens being connected with interception pipeline L24-L16 for the current chromatographic column Z1 for exporting efflux A
Output pipe two-port valve V124 and latter root chromatogram column Z2 with the intake line two-port valves that are connected of interception pipeline L24-L16
V216 opens interception pipeline, simultaneously closes off chromatographic column Z1 efflux A circulation line T1, formed chromatographic column Z1 and chromatographic column Z2 it
Between efflux A return lines；
It is similarly set in interception pipeline L23-L15 and L22-L14, forms the efflux between chromatographic column Z3 and chromatographic column Z4
Efflux C return lines between B return lines and chromatographic column Z7 and chromatographic column Z8；
1 mobile phase delivery pump P3 in pipeline L21-L13 is intercepted is set, opens current output A, B mixture efflux
Chromatographic column Z5 with interception pipeline L21-L13 the output pipe two-port valve V521 that is connected and chromatographic column Z3 with intercepting pipeline
The intake line two-port valve V313 that L21-L13 is connected, the efflux AB's formed between chromatographic column Z5 and chromatographic column Z3 bypasses
Pipeline.
The operating mode of the device is specially：
Z1：V112 and V124 are opened, and with eluent D elution fraction A, stationary phase regeneration, a component A effluxes part flows into storage
Flow container A, a part are back to Z2 by return line L24-L16；
Z2：V216 and T2 are opened, and component A is finely detached with B；
Z3：V313 and V323 are opened, and component A, B is adsorbed and detached, and component A, B mixed liquor is carried by bypassing pipeline L21-L13
For a component B effluxes part flows into fluid reservoir B, and a part is back to Z4 by return line L23-L15；
Z4：V415 and T4 are opened, and recycle component B, mobile phase regeneration；
Z5：V521 and T5 are opened, elution fraction A, B mixture, stationary phase regeneration, A, B mixture efflux part pass through around
It crosses pipeline L21-L13 and flows into Z3, a part is back to Z6 by return line L23-L15；
Z6：T6 is opened, and component A, B mixture and component C are finely detached；
Z7：V711 and V722 are opened, and A, B, C of material liquid are adsorbed and detached, and a component C effluxes part flows into fluid reservoir
C, a part are back to Z8 by return line L22-L14；
Z8：V814 and T8 are opened, and recycle component C, mobile phase regeneration.
When reaching switching time, operating mode is moved to next root chromatogram column in circuit by control system along mobile phase direction,
The process is repeated, and the move counter-current for simulating stationary phase and mobile phase flows, and by adsorption and desorption and rectifying, realizes 3 groups
Separation.
Simulation moving bed device shown in Fig. 2 is specially：If there are one circuit, six zone, 1-1-2-1-1-2, separation
Three component A, B and C.
It is sealed in the outlet for more being passed through mouth and threeway using plug, closes the pipeline Ln14 and L22- unrelated with operating mode
14, while the outlet of former L23-L15 interception pipeline threeways is sealed with plug, convey D2 eluents with P5.
The operating mode of the device is specially：
Z1：V112 and V124 are opened, and with eluent D1 elution fraction A, stationary phase regeneration, a component A effluxes part flows into
Fluid reservoir A, a part are back to Z2 by return line L24-L16；
Z2：V216 and T2 are opened, and component A is finely detached with B；
Z3 and Z4：V313, T3 and V423 are opened, and component A, B is adsorbed and detached, and component A, B mixed liquor is by bypassing pipeline
L21-L13 is provided, and component B effluxes flow into fluid reservoir B；
Z5：V515, V521 and T5 are opened, with D2 elution fraction A and B, stationary phase regeneration, an A and B mixtures efflux part
Z3 is flowed into through bypassing pipeline, a part is recycled to Z6；
Z6：T6 is opened, and component A, B mixture and component C are finely detached；
Z7 and Z8：V711, T7 and V822 are opened, and A, B, C of material liquid are adsorbed and detached, and component C effluxes flow into liquid storage
Tank C.
When reaching switching time, operating mode is moved to next root chromatogram column in circuit by control system along mobile phase direction,
The process is repeated, and the move counter-current for simulating stationary phase and mobile phase flows, and by adsorption and desorption and rectifying, realizes 3 groups
Separation.
Simulation moving bed device shown in Fig. 3 is specially：If there are one circuit, tetra- zone of 2-2-2-2 detach two components
A、B。
The operating mode of the device is specially：
Z1 and Z2：V112, T1, V224 are opened, with eluent D elution fraction A, stationary phase regeneration, a component A effluxes part
Fluid reservoir A is flowed into, a part is back to Z3 by return line L24-L16；
Z3 and Z4：V316, T3, T4 are opened, and component A is finely detached with B；
Z5 and Z6：V511, T5 and V623 are opened, and component A, B is adsorbed and detached, and a component B effluxes part flows into liquid storage
Tank B, a part are back to Z7 by return line L23-L15；
Z7 and Z8：V715, T7 and T8 are opened, and recycle component B, mobile phase regeneration；
When reaching switching time, operating mode is moved to next root chromatogram column in circuit by control system along mobile phase direction,
The process is repeated, and the move counter-current for simulating stationary phase and mobile phase flows, and by adsorption and desorption and rectifying, realizes 2 groups
Separation.
For tetra- zone of 2-2-2-2, divide t1, t2, t3, t4 period successively switching cycle Ts,
t1：Component B is exported, next root chromatogram column, switching cycle Ts are moved to along mobile phase direction；
t2：By eluent entrance, next root chromatogram column, switching cycle Ts are moved to along mobile phase direction；
t3：Component A is exported, next root chromatogram column, switching cycle Ts are moved to along mobile phase direction；
t4：By feed inlet, next root chromatogram column, switching cycle Ts are moved to along mobile phase direction；
Ts：It restores, tetra- zone of 2-2-2-2.
The above process repeats, and thus asynchronised handover changes each band chromatographic column number, that is, zone length.
Simulation moving bed device shown in Fig. 4 is specially：One circuit of setting, six zone, 1-1-2-1-1-2, wherein
First band independence and gradient elution detach three component A, B and C.
Eluent D1 is pumped into input bus L12 in fluid reservoir D1 by infusion pump P2, eluent D2 in fluid reservoir D2 by
Infusion pump P4 is pumped into input bus L14, and eluent D3 is pumped into input bus L15, eluent in fluid reservoir D3 by infusion pump P5
D4 is pumped into input bus L16 in fluid reservoir D4 by infusion pump 6；The threeway original interception pipeline of L24, L23, L22 output bus goes out
It is sealed at mouthful with plug.
Operating mode is specially：
Z1：V112, V114 and V124 are opened, with eluent D1 and D2 gradient elution component A, stationary phase regeneration, component A outflows
Liquid stream enters fluid reservoir A；
Z2：V215 and T2 are opened, and make mobile phase, fine separation component A and B with D3；
Z3 and Z4：V313, T3 and V423 are opened, and component A, B is adsorbed and detached, and component A, B mixed liquor is by bypassing pipeline
L21-L13 is provided, and component B effluxes flow into fluid reservoir B；
Z5：V516, V521 and T5 are opened, with D4 elution fraction A and B, stationary phase regeneration, an A and B mixtures efflux part
Z3 is flowed into through bypassing pipeline, a part is recycled to Z6；
Z6：T6 is opened, and component A, B mixture and component C are finely detached；
Z7 and Z8：V711, T7 and V822 are opened, and mixture A, B, C are adsorbed and detached, and component C effluxes flow into fluid reservoir
C。
Simulation moving bed device shown in fig. 5 is specially：Setting Z1~Z4, totally 4 root chromatogram columns participate in separation, perform sequence
Chromatographic isolation, each band independent operating can carry out four sections of fraction As of separation, B, C and W or carry out gradient elution.
Eluent D1 is pumped into input bus L12 in fluid reservoir D1 by infusion pump P2, eluent D2 in fluid reservoir D2 by
Infusion pump P3 is pumped into input bus L13, and eluent D3 is pumped into input bus L14 in fluid reservoir D3 by infusion pump P4；Respectively by
L24, L23, L22 and L21 export component A to fluid reservoir A, component B to fluid reservoir B, component C to fluid reservoir C and component W to liquid storage
Tank W；It is sealed at the threeway original interception tube outlet of L24, L23, L22 output bus with plug
Operating mode is specially：
Z1：V114, V124 are opened, and with eluent D1 elution fraction A, stationary phase regeneration, component A effluxes flow into fluid reservoir A；
Z2：V213 and V223 are opened, and make mobile phase, fine separation component B with D2；
Z3：V312 and V322 are opened, and make mobile phase, fine separation component C with D3；
Z4：V411 and V421 are opened, and component A, B, C, W into sample liquid are adsorbed and detached, and W effluxes flow into fluid reservoir B；
Simulation moving bed device shown in fig. 6 is specially that " fried dough twist formula " tail head of chromatographic column is connected.
Here only consider the set-up mode of chromatography intercolumniation circulation line, do not consider working condition.8 root chromatogram columns are arranged in order
Serial number：Z1, Z2, Z3, Z4, Z5, Z6, Z7, Z8, setting N root chromatogram columns participate in separation process, chromatography when 3≤N≤8, N=8
The connection mode of column is：Z1, Z3, Z5, Z7, Z8, Z6, Z4, Z2, Z1, i.e.,：Both ends Z7 is connected with Z8 tails head, Z2 and Z1 tail prime ministers
Even, other interval chromatographic column tail head are connected, and form the circuit of 8 root chromatogram columns；When selection participates in the chromatographic column number of separation, this
Kind circulation line is isometric, and connection mode is easy to operate, such as：It is converted to as N=6 or by the connection mode of chromatographic column during N=8
During N=6, Z5 circulation lines are connected in Z6 arrival ends, link circuit is：Z1, Z3, Z5, Z6, Z4, Z2, Z1, i.e.,：Both ends Z5
Be connected with Z6 tails head, Z2 is connected with Z1 tails head, other interval chromatographic column tail head are connected, form 6 root chromatogram columns circuit；Work as N=7
When or when the connection mode of chromatographic column during N=8 is converted to N=7, Z6 circulation lines are connected in Z7 arrival ends, are connected back to
Lu Wei：Z1, Z3, Z5, Z7, Z6, Z4, Z2, Z1, i.e.,：Both ends Z7 is connected with Z6 tails head, Z2 is connected with Z1 tails head, other interval colors
Spectrum column tail head is connected, and forms the circuit of 7 root chromatogram columns；
By the setting of this circulation line, can the device of the present embodiment readily be formed into more set moving beds, for example,
During N=8, Z3 circulation lines are connected in Z4 arrival ends, Z6 circulation lines are connected in Z5 arrival ends, you can form two sets of each 4 columns
Moving bed, it (can be different mobile phases, different stationary phase, different former that two sets of moving bed systems, which can be arranged to independent operating,
Feed liquid), parallel running or series operation.
Simulation moving bed device shown in Fig. 7 is specially：" fried dough twist formula " tail head of chromatographic column is connected, two 1-1-2 simulations
Moving bed circuit, separation component A, B and C.
Eluent D1 is pumped into input bus L12 in fluid reservoir D1 by infusion pump P2, eluent D2 in fluid reservoir D2 by
Infusion pump P5 is pumped into input bus L15.It is sealed at the threeway original interception tube outlet of L23, L22 output bus with plug.
Operating mode is specially：
The first circuit order of connection is：Z1, Z3, Z4, Z2 and Z1；
Z1：V112 and V124 are opened, and with eluent D1 elution fraction A, stationary phase regeneration, a component A effluxes part flows into
Fluid reservoir A, a part are back to Z3 through return line L24-L16；
Z3：V316 and T3 are opened, and component A is finely detached with B；
Z4 and Z2：V413, T4 and V223 are opened, and component A, B is adsorbed and detached, and component A, B mixed liquor is by bypassing pipeline
L21-L13 is provided, and component B effluxes flow into fluid reservoir B；
The second circuit order of connection is：Z5, Z7, Z8, Z6 and Z5.
Z5：V515, V521 and T5 are opened, with D2 elution fraction A and B, stationary phase regeneration, an A and B mixtures efflux part
Z4 is flowed into through bypassing pipeline, a part is recycled to Z7；
Z7：T7 is opened, and component A, B mixture and component C are finely detached；
Z8 and Z6：V811, T8 and V622 are opened, and mixture A, B, C are adsorbed and detached in material liquid, component C outflow liquid streams
Enter fluid reservoir C.
The connecting line between 2 sets of Simulation moving beds is disconnected, may be constructed 3~7 sets of Simulation moving bed control systems, is equipped with
Pump, pipeline, threeway and fluid reservoir carry out 4-14 component separation.
Claims (8)
1. a kind of Simulation moving bed device, including M root chromatogram columns, which is characterized in that 4≤M≤30 per root chromatogram column entrance and go out
Connection entrance is mostly logical respectively and outlet is mostly logical for mouth, and the more reduction of fractions to a common denominators of entrance do not connect following for 6 intake lines and previous root chromatogram column
Endless tube road exports more reduction of fractions to a common denominators and does not connect 4 output pipes and the circulation line of current chromatographic column；The every intake line
Or output pipe connects respectively with corresponding input bus or output bus；Material liquid, eluent are total by inputting accordingly respectively
Line the input phase answers the intake line of chromatographic column；The circulation line connects the previous more logical and current chromatographic columns in root chromatogram column outlet
Entrance is mostly logical, and all chromatographic columns is made to pass through circulation line tail head and are connected；Various column effluents in addition to efflux is recycled
Corresponding output bus is output to by corresponding output pipe by corresponding chromatographic column respectively；
Material liquid, eluent are stored in corresponding fluid reservoir；The various column effluents flowed out from output bus are simulated
The system efflux of moving bed is stored in corresponding fluid reservoir；
Two-port valve is respectively provided on intake line, output pipe and circulation line per root chromatogram column；The two-port valve is by solenoid valve
It is formed with check (non-return) valve, and each two-port valve is controlled to be turned on and off state by PLC or single-chip computer control system；
The chromatographic column works under the constant temperature in the range of -10 DEG C~200 DEG C；
Wherein, the chromatographic column of separation process is participated in said device as N roots, and 3≤N≤M, N root chromatogram columns pass through circulation line
Tail head is connected, forming circuit；
Also, an output bus with an input bus is connect, forms interception pipeline.
2. a kind of Simulation moving bed device according to claim 1, which is characterized in that open the color of current output efflux
Spectrum column with the latter root chromatogram column of the output pipe two-port valve that is connected of interception pipeline and the column and the interception pipeline
Connected intake line two-port valve forms return line, and delivery pump is set on return line；
Or 1 threeway and 1 delivery pump are set in pipeline is intercepted, a mouth of the threeway is for exporting efflux, together
When open current output efflux chromatographic column the output pipe two-port valve being connected with the interception pipeline and the column it is latter
The intake line two-port valve being connected with the interception pipeline of root chromatogram column, equally constitutes return line；
Also, above two is formed in the mode of return line, when the return line of current chromatographic column is opened, by current chromatography
Column circulation line is closed.
3. a kind of Simulation moving bed device according to claim 1, which is characterized in that open the color of current output efflux
The output pipe two-port valve being connected with the interception pipeline of spectrum column and any one color in addition to the latter root chromatogram column of the column
The intake line two-port valve being connected with the interception pipeline of spectrum column, is formed around pipeline；
Described bypass sets 0~1 delivery pump in pipeline.
4. a kind of Simulation moving bed device according to claim 1, which is characterized in that for same operating mode,
In switching cycle, import, outlet port are set by control system time segment, adjust i.e. each band of length of each functional areas band
Chromatographic column number.
A kind of 5. Simulation moving bed device according to any one in Claims 1 to 4, which is characterized in that the M roots
The serial number that chromatographic column is arranged in order：Z1, Z2, Z3, Z4, Z5 ..., Z (n-1), Zn, Z (n+1) ..., ZM, then in the N roots
In chromatographic column, the adjacent chromatographic column tail head for coming both ends is connected, and other chromatographic column tail head separately are connected, chromatographic column tail prime minister
It is even the circulation line, all circulation lines are isometric；
When N is even number, the connection mode of N root chromatogram columns is：Z1、Z3、Z5、…、Z(N-3)、Z(N-1)、ZN、Z(N-2)、Z(N-
4) ..., Z4, Z2, Z1, i.e.,：By the increased direction of odd number, odd number chromatographic column tail prime minister is connected to one end Z (N-1), Z (N-1) and ZN
Tail head is connected, and then, reduces direction by even number, even number chromatographic column tail prime minister is connected to other end Z2, Z2 and Z1 tail head and is connected, and forms
The circuit of N root chromatogram columns is connected for " fried dough twist formula " tail head；
When N is odd number, ZN is connected with Z (N-1) tails head, other identical with N is even number situation.
6. according to a kind of Simulation moving bed device described in claim 1, which is characterized in that the simulation of N root chromatogram columns is moved
Dynamic bed is decomposed into 2 sets of Simulation moving bed systems, i.e.,：L root chromatogram column tails head is connected to form a set of Simulation moving bed, 3≤L≤(N-
3), residue (N-L) root chromatogram column tail head is connected to form other set Simulation moving bed, and 2 sets of Simulation moving bed systems are transported to be independent
Row pattern, parallel running mode or series operation pattern.
7. a kind of Simulation moving bed device according to claim 1, which is characterized in that all chromatographic columns are set to one
Region, all two-port valves are set to another region, and temperature control is carried out to chromatography columnar region.
8. a kind of Simulation moving bed device according to claim 1, which is characterized in that on input bus be equipped with filter,
On-line degassing machine is equipped with flowmeter on circulation line, the detector of flowmeter, solution concentration and purity is equipped on output bus.
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| CN108840793B (en) * | 2018-05-28 | 2021-06-15 | 辽宁科技大学 | Method for preparing gamma-thujaplicin by using simulated moving bed chromatography |
| JP7225024B2 (en) * | 2018-11-16 | 2023-02-20 | オルガノ株式会社 | Simulated moving bed chromatographic separation method and simulated moving bed chromatographic separation system |
| US11839835B2 (en) | 2018-11-16 | 2023-12-12 | Organo Corporation | Simulated moving-bed type chromatographic separation method and simulated moving-bed type chromatographic separation system |
| CN109738550B (en) * | 2019-02-25 | 2024-04-16 | 青岛众瑞智能仪器股份有限公司 | Continuous purification experimental device |
| CN110665256B (en) * | 2019-10-08 | 2021-01-08 | 中国科学院过程工程研究所 | Simulated moving bed device and method for separating multicomponent dihydric alcohol |
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| CA2139033C (en) * | 1993-12-27 | 2004-04-20 | Masatake Tanimura | Method of separation into three components using a simulated moving bed |
| CN101732890A (en) * | 2009-12-08 | 2010-06-16 | 辽宁科技大学 | Three-section simulated moving bed chromatography device |
| CN105617714A (en) * | 2015-12-31 | 2016-06-01 | 厦门大学 | Asynchronous switching three-zone-belt simulation moving bed |
| CN206334397U (en) * | 2016-09-19 | 2017-07-18 | 辽宁科技大学 | A kind of moving bed imitation chromatogram separation facility |
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| CA2139033C (en) * | 1993-12-27 | 2004-04-20 | Masatake Tanimura | Method of separation into three components using a simulated moving bed |
| CN101732890A (en) * | 2009-12-08 | 2010-06-16 | 辽宁科技大学 | Three-section simulated moving bed chromatography device |
| CN105617714A (en) * | 2015-12-31 | 2016-06-01 | 厦门大学 | Asynchronous switching three-zone-belt simulation moving bed |
| CN206334397U (en) * | 2016-09-19 | 2017-07-18 | 辽宁科技大学 | A kind of moving bed imitation chromatogram separation facility |
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