CN106166402A - A kind of moving bed imitation chromatogram separation facility - Google Patents
A kind of moving bed imitation chromatogram separation facility Download PDFInfo
- Publication number
- CN106166402A CN106166402A CN201610832972.6A CN201610832972A CN106166402A CN 106166402 A CN106166402 A CN 106166402A CN 201610832972 A CN201610832972 A CN 201610832972A CN 106166402 A CN106166402 A CN 106166402A
- Authority
- CN
- China
- Prior art keywords
- moving bed
- column
- chromatographic column
- root chromatogram
- simulation moving
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- 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
-
- 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
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Treatment Of Liquids With Adsorbents In General (AREA)
Abstract
Present invention aims to the problems such as existing SMB equipment operating mode is more fixing, it is provided that a kind of moving bed imitation chromatogram separation facility, belong to technical field of chromatography separation.This device is made up of 8～30 root chromatogram columns, every root chromatogram column is controlled 6 intake lines, 4 output pipes and 1 circulation line by 11 two-port valves, the respective duty of all two-port valves is controlled by PLC or single-chip computer control system, multiple mode of operation can be set, including: the chromatographic column number participating in separating is set, multi-zone is set, intercepting pipeline is set, setting area interband is continuously or independent operating process, arranging either synchronously or asynchronously switch mode, this device pipeline is easy to connect, flexible operation, easily safeguard, it is possible to complete multicomponent separation.
Description
Technical field
The invention belongs to technical field of chromatography separation, particularly to a kind of general-purpose simulation mobile bed chromatic segregation apparatus.
Background technology
Simulated moving bed chromatography (being called for short SMB) technology has high separation, high yield, high yield, high efficiency and company
Continuous automatic running scheme, is high-end separation means.Simulated movable bed chromatography device is connected into closed circuit by some tail prime ministers
Chromatographic column forms, and carrys out mould by regularly moving the position of flowing phase import and effluent outlet along the flow direction of flowing phase
Intend the fixing move counter-current flowing with flowing phase, and then realize the separation of different component.SMB mode of operation includes arranging participation
Separate chromatographic column number, divide difference in functionality district, each district chromatographic column is set, simulated moving bed chromatography separation principle determines work
The multiformity of operation mode；And mode of operation is that Optimized Simulated mobile bed chromatic separates the key factor first examined or check, but actual
On SMB equipment mostly by switching valve and software kit restrict use more fix operational mode, same SMB equipment
It is difficult to realize the conversion between multiple different mode.
Summary of the invention
The present invention provides a kind of general-purpose simulation mobile bed chromatic segregation apparatus.This device is each chromatograph in SMB system
Post arranges 11 two-port valves, can arrange multiple mode of operation, it is achieved multicomponent separation.
A kind of simulation moving bed device, including M root chromatogram column, 4≤M≤30, every root chromatogram column entrance and exit connects respectively
Access port manifold and outlet manifold, entrance manifold connects 6 intake lines and the circulation line of previous root chromatogram column respectively, goes out
Mouth manifold connects 4 output pipes and the circulation line of current chromatographic column respectively；Every described intake line or outlet tube
Road connects with corresponding input bus or output bus respectively；Material liquid, eluent are inputted phase by corresponding input bus respectively
Answer the intake line of chromatographic column；Described circulation line connects previous root chromatogram column outlet manifold and current chromatograph column inlet is many
Logical, make all chromatographic columns be connected by circulation line tail head；Except circulation effluent in addition to various column effluent respectively by
Corresponding chromatographic column exports corresponding output bus by corresponding output pipe；
Material liquid, eluent are stored in corresponding fluid reservoir；The various column effluent flowed out from output bus are
The system effluent of simulation moving bed is stored in corresponding fluid reservoir；
It is respectively provided with two-port valve on every intake line of root chromatogram column, output pipe and circulation line；Described two-port valve is by electricity
Magnet valve and check (non-return) valve composition, and controlled each two-port valve for being turned on and off state by PLC or single-chip computer control system；
Described chromatographic column works under the constant temperature in the range of-10 DEG C～200 DEG C；
Above-mentioned simulation moving bed device, can arrange multi-zone SMB: such as three band a-b-c, four band SMB:a-b-c-d, and five
Band SMB:a-b-c-d-e six band refers to often band chromatographic column number to more bands, a, b, c, d, e, can arrange open loop input material liquid
Or the pattern of eluent pattern, adsorption zone and slow component fine separation district are continuous, the pattern of elution zone independence, each district independence work
The order SMB operational mode made.
Further, above-mentioned simulation moving bed device, optional SMB participates in the chromatographic column number separated, it may be assumed that described
The chromatographic column participating in separation process in device is N root, 3≤N≤M；N root chromatogram column is connected by circulation line tail head, is formed back
Road.
Further, above-mentioned simulation moving bed device, an output bus and an input bus are connected, constitutes and cut
Take pipeline.
Further, above-mentioned simulation moving bed device, it is possible to achieve intercept part effluent and continuous backflow refines, beat
Open the output pipe two-port valve being connected with described intercepting pipeline and a rear color of this post of the chromatographic column of current output effluent
The intake line two-port valve being connected with described intercepting pipeline of spectrum post, constitutes reflux pipe, and arranges defeated on reflux pipe
Send pump；
Or arranging 1 threeway and 1 delivery pump in intercepting pipeline, a mouth of described threeway is used for exporting outflow
Liquid, opens the output pipe two-port valve being connected with described intercepting pipeline of the chromatographic column of current output effluent and this post simultaneously
The intake line two-port valve being connected with described intercepting pipeline of a rear root chromatogram column, equally constitutes reflux pipe；
Further, above two constitutes in the mode of reflux pipe, when the reflux pipe of current chromatographic column is opened, and will be current
Chromatographic column circulation line is closed.
Or, above-mentioned simulation moving bed device, it is possible to achieve intercept part effluent and feed back to sample introduction entrance or wash
De-liquid entrance, opens the output pipe two-port valve being connected with described intercepting pipeline of the chromatographic column of current output effluent and except being somebody's turn to do
The intake line two-port valve being connected with described intercepting pipeline of any one root chromatogram column outside a rear root chromatogram column of post, constitute around
Cross pipeline；
Described walking around arranges 0～1 delivery pump in pipeline.
Further, above-mentioned simulation moving bed device, either synchronously or asynchronously switch mode can be set, for same work
Operation mode, in switching cycle, arranges import, exit position by control system time segment, adjusts each function zone
Length the most each band chromatographic column number.
Further, above-mentioned simulation moving bed device, the serial number that described M root chromatogram column is arranged in order: Z1, Z2,
Z3, Z4, Z5 ..., Z (n-1), Zn, Z (n+1) ..., ZM, then, in described N root chromatogram column, come the adjacent chromatographic column at two ends
Tail head is connected, and other chromatographic column tail head separately is connected, and chromatographic column tail head is connected and is described circulation line, all circulation pipes
Road is isometric；
When N is even number, the connected mode of N root chromatogram column is: Z1, Z3, Z5 ..., Z (N-3), Z (N-1), ZN, Z (N-2), Z
(N-4) ..., Z4, Z2, Z1, it may be assumed that by odd number increase direction, odd number chromatographic column tail prime minister be connected to one end Z (N-1), Z (N-1) with
ZN tail head is connected, and then, reduces direction by even number, and even number chromatographic column tail prime minister is connected to other end Z2, Z2 and Z1 tail head and is connected, structure
Become the loop of N root chromatogram column, be connected for " Flos Cannabis formula " tail head；
When N is odd number, the connected mode of N root chromatogram column is: Z1, Z3, Z5 ..., Z (N-4), Z (N-2), ZN, Z (N-1), Z
(N-3) ..., Z4, Z2, Z1, it may be assumed that by odd number increase direction, odd number chromatographic column tail prime minister is connected to one end ZN, ZN and Z (N-1) tail
First connected, then, reduce 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 constitutes N
The loop of root chromatogram column, is connected for " Flos Cannabis formula " tail head；
The mode using " Flos Cannabis formula " tail head to be connected connects pipeline, it is possible to make the liquid circulated of circulation line have approximation
Course of conveying, it is to avoid differential diffusion.
Further, above-mentioned simulation moving bed device, the arrangement mode of described M root chromatogram column is word order, annular
During the modes such as arrangement or rectangular arranged, " Flos Cannabis formula " tail head is connected convenient, and pipeloop is isometric.
Further, above-mentioned simulation moving bed device, multiple-working mode can be set and work simultaneously, by N root chromatogram column
Simulation moving bed be decomposed into 2 sets simulation moving bed systems, it may be assumed that L root chromatogram column tail head is connected to form a set of simulation moving bed, 3
≤ L≤(N-3), residue (N-L) root chromatogram column tail head are connected to form other set simulation moving bed, 2 set simulation moving bed systems
For independent operation mode, parallel running mode or series operation pattern.
Further, above-mentioned simulation moving bed device, disconnect the connection pipeline between 2 set simulation moving beds, it is possible to structure
Becoming number set difference simulation moving bed system, number set simulation moving bed system is independent operation mode, parallel running mode or string
Through transport row mode.
Further, above-mentioned simulation moving bed device, all chromatographic columns are arranged at a region, all two-port valves set
It is placed in another one region, chromatograph columnar region is carried out temperature control.
Further, above-mentioned simulation moving bed device, input bus is equipped with filter, online degasser, circulation pipe
It is equipped with effusion meter on road, output bus is equipped with effusion meter, solution concentration and the detector of purity.
Further, above-mentioned simulation moving bed device, the pipeline unrelated with mode of operation all can in corresponding manifold or
Seal with plug at threeway, to extend the relevant two-port valve life-span.
Compared with prior art, present invention have an advantage that
1, this device has several functions: arrange the chromatographic column number that SMB participates in separating；Multi-zone SMB is set: such as three bands
A-b-c, four band SMB:a-b-c-d, multicolored vaginal discharge SMB:a-b-c-d-e, six band are to more bands, and a, b, c, d refer to often band chromatographic column number；
Setting area interband runs or independent operation mode continuously；The pattern of open loop sample introduction and sampling is set；Arrange and either synchronously or asynchronously switch
Pattern；Intercept part effluent and feed back to sample introduction entrance or eluent entrance；Multiple-working mode works simultaneously；Complete many groups
Divide separation etc..
2, two-port valve flexible operation, easily safeguards.
3, pipeline is easy to connect.
4, valve is placed with chromatographic column subregion, can be to chromatographic column entirety temperature control.
Accompanying drawing explanation
Fig. 1 is the simulation moving bed device schematic diagram of a kind of 8 root chromatogram columns, and this simulation moving bed is a loop, eight
Zone, 1-1-1-1-1-1-1-1, separate three strong absorbed component A of component, intermediate adsorption component B and weakly adsorbed components C.
Fig. 2 is the simulation moving bed device schematic diagram of a kind of 8 root chromatogram columns, and this simulation moving bed is a loop, six
Zone, 1-1-2-1-1-2, separate three components A, B and C.The pipeline unrelated with mode of operation can be at corresponding manifold or threeway
Seal with plug.
Fig. 3 is the simulation moving bed device schematic diagram of a kind of 8 root chromatogram columns, and this simulation moving bed is a loop, four
Zone, 2-2-2-2, separate two components A, B.
Fig. 4 is the simulation moving bed device schematic diagram of a kind of 8 root chromatogram columns, and this simulation moving bed is a loop, six
Zone, 1-1-2-1-1-2, wherein the first band independence and gradient elution, separate three components A, B and C.
Fig. 5 is the simulation moving bed device schematic diagram of a kind of 8 root chromatogram columns, execution sequence chromatographic isolation, 4 root chromatogram column ginsengs
With separate, each band independent operating, or separate four sections of fraction A, B, C and W, or use gradient elution.
Fig. 6 is the simulation moving bed device schematic diagram of a kind of 8 root chromatogram columns, and this simulation moving bed is " Flos Cannabis formula " tail prime minister
Even.
Fig. 7 is the simulation moving bed device schematic diagram of a kind of 8 root chromatogram columns, and this simulation moving bed is " Flos Cannabis formula " tail prime minister
Even, two 1-1-2 simulate moving bed loop, separation component A, B and C.
Wherein, the Zn: the n-th root chromatogram column, n: chromatographic column sequence number, Lmi: input or output bus, m=1 represents input, m=2
Representing output, i is input or output bus sequence number, the Lnmi: the n-th root chromatogram column input/output pipeline；The two-way of Vnmi:Lnmi
Valve, Tn: circulation line two-port valve；
F: material liquid fluid reservoir, D or Dq: eluent D or eluent Dq fluid reservoir, q: eluent sequence number, A: separation component A
Fluid reservoir, B: component B fluid reservoir, C: component C fluid reservoir, W: component W fluid reservoir, the delivery pump of Pi: the i-th input bus.
Detailed description of the invention
With 8 root chromatogram column simulation moving bed devices, for 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 exit connects respectively
Access port manifold and outlet manifold, entrance manifold connects the circulation line T (n-of 6 intake lines and previous root chromatogram column respectively
1), outlet manifold connects the circulation line Tn of 4 output pipes and current chromatographic column, totally 11 pipelines respectively；Material liquid, eluting
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 entrance, makes all chromatographic column tail head be connected；Various chromatographic columns in addition to circulation effluent
Effluent imports corresponding output bus via respective output pipe respectively；Material liquid, eluent are stored in corresponding liquid storage
In tank；The system effluent i.e. simulating moving bed from the solution of output bus outflow 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 at room temperature works；Two-way
Valve is made up of electromagnetic valve and check (non-return) valve, PLC or single-chip computer control system control the respective duty of all two-port valves, or open
Or close.Carrying out practically step is embodied by the open and close state of each two-port valve, here, only describe the opening state of chromatographic column, closes
Closed state does not repeats, and the Tn that chromatographic column circulation line two-port valve is only arranged with Way out represents.
Simulation moving bed device shown in Fig. 1 particularly as follows: be provided with a loop, eight zone, 1-1-1-1-1-1-1-1,
Separate three components, the strongest absorbed component A, intermediate adsorption component B and weakly adsorbed components C；
In the apparatus, material liquid is pumped into input bus L11 by infusion pump P1 in fluid reservoir F, and eluent is in fluid reservoir D
In pumped into input bus L12 by infusion pump P2, after separation, component A enters fluid reservoir A through output bus L24, and component B is total through output
Line L23 enters fluid reservoir B, and component C enters fluid reservoir C through output bus L22；
Connect an output bus therein and an input bus therein, constitute and intercept pipeline, L24-L16, L23-
L15、L22-L14、L21-L13；
One threeway and a flowing phase delivery pump P6 are set in intercepting pipeline L24-L16, a mouth output of threeway
The system effluent A of this intercepting pipeline, opens being connected with intercepting pipeline L24-L16 of current chromatographic column Z1 exporting effluent A
An output pipe two-port valve V124 and rear root chromatogram column Z2 with intercept the intake line two-port valve that is connected of pipeline L24-L16
V216, opens intercepting pipeline, simultaneously closes off chromatographic column Z1 effluent A circulation line T1, formed chromatographic column Z1 and chromatographic column Z2 it
Between effluent A reflux pipe；
In like manner arrange intercepting pipeline L23-L15 and L22-L14, form the effluent between chromatographic column Z3 and chromatographic column Z4
B reflux pipe, and the effluent C reflux pipe between chromatographic column Z7 and chromatographic column Z8；
1 flowing phase delivery pump P3 is set in intercepting pipeline L21-L13, opens and currently export A, B mixture effluent
Chromatographic column Z5 with intercept the output pipe two-port valve V521 that is connected of pipeline L21-L13 and chromatographic column Z3 with intercept pipeline
The intake line two-port valve V313 that L21-L13 is connected, forms walking around of the effluent AB between chromatographic column Z5 and chromatographic column Z3
Pipeline.
The mode of operation of this device particularly as follows:
Z1:V112 and V124 opens, and with eluent D elution fraction A, fixes and regenerates mutually, and a component A effluent part flows into storage
Flow container A, a part is back to Z2 by reflux pipe L24-L16；
Z2:V216 and T2 opens, component A and B fine separation；
Z3:V313 and V323 opens, and component A, B are adsorbed and separate, and component A, B mixed liquor are carried by walking around pipeline L21-L13
Confession, a component B effluent part flows into fluid reservoir B, and a part is back to Z4 by reflux pipe L23-L15；
Z4:V415 and T4 opens, and reclaims component B, and flowing regenerates mutually；
Z5:V521 and T5 opens, elution fraction A, B mixture, fixing regenerates mutually, A, B mixture effluent part through around
Crossing pipeline L21-L13 and flow into Z3, a part is back to Z6 by reflux pipe L23-L15；
Z6:T6 opens, component A, B mixture and component C fine separation；
Z7:V711 and V722 opens, and A, B, C of material liquid are adsorbed and separate, and a component C effluent part flows into fluid reservoir
C, a part is back to Z8 by reflux pipe L22-L14；
Z8:V814 and T8 opens, and reclaims component C, and flowing regenerates mutually.
When arriving switching time, mode of operation is moved to next root chromatogram column in loop along flowing phase direction by control system,
This process is repeated, and the fixing move counter-current flowing with flowing phase of simulation, through adsorption and desorption and rectification, it is achieved 3 groups
Separate.
Simulation moving bed device shown in Fig. 2 particularly as follows: be provided with a loop, six zone, 1-1-2-1-1-2, separate
Three components A, B and C.
Outlet in manifold entrance and threeway uses plug to seal, and closes pipeline Ln14 and L22-unrelated with mode of operation
14, the outlet plug that former L23-L15 intercepts pipeline threeway simultaneously seals, and carries D2 eluent with P5.
The mode of operation of this device particularly as follows:
Z1:V112 and V124 opens, and with eluent D1 elution fraction A, fixes and regenerates mutually, and a component A effluent part flows into
Fluid reservoir A, a part is back to Z2 by reflux pipe L24-L16；
Z2:V216 and T2 opens, component A and B fine separation；
Z3 and Z4:V313, T3 and V423 open, and component A, B are adsorbed and separate, and component A, B mixed liquor are by walking around pipeline
L21-L13 provides, and component B effluent flows into fluid reservoir B；
Z5:V515, V521 and T5 open, and with D2 elution fraction A and B, fix and regenerate mutually, an A and B mixture effluent part
Flowing into Z3 through walking around pipeline, a part is recycled to Z6；
Z6:T6 opens, component A, B mixture and component C fine separation；
Z7 and Z8:V711, T7 and V822 open, and A, B, C of material liquid are adsorbed and separate, and component C effluent flows into liquid storage
Tank C.
When arriving switching time, mode of operation is moved to next root chromatogram column in loop along flowing phase direction by control system,
This process is repeated, and the fixing move counter-current flowing with flowing phase of simulation, through adsorption and desorption and rectification, it is achieved 3 groups
Separate.
Simulation moving bed device shown in Fig. 3 particularly as follows: be provided with a loop, tetra-zone of 2-2-2-2, separate two components
A、B。
The mode of operation of this device particularly as follows:
Z1 and Z2:V112, T1, V224 open, and with eluent D elution fraction A, fix and regenerate mutually, a component A effluent part
Flowing into fluid reservoir A, a part is back to Z3 by reflux pipe L24-L16；
Z3 and Z4:V316, T3, T4 open, component A and B fine separation；
Z5 and Z6:V511, T5 and V623 open, and component A, B are adsorbed and separate, and a component B effluent part flows into liquid storage
Tank B, a part is back to Z7 by reflux pipe L23-L15；
Z7 and Z8:V715, T7 and T8 open, and reclaim component B, and flowing regenerates mutually；
When arriving switching time, mode of operation is moved to next root chromatogram column in loop along flowing phase direction by control system,
This process is repeated, and the fixing move counter-current flowing with flowing phase of simulation, through adsorption and desorption and rectification, it is achieved 2 groups
Separate.
For tetra-zone of 2-2-2-2, divide t1, t2, t3, t4 time period successively switching cycle Ts,
T1: component B exported, moves to next root chromatogram column along flowing phase direction, and switching cycle is Ts；
T2: by eluent entrance, moving to next root chromatogram column along flowing phase direction, switching cycle is Ts；
T3: component A exported, moves to next root chromatogram column along flowing phase direction, and switching cycle is Ts；
T4: by charging aperture, moving to next root chromatogram column along flowing phase direction, switching cycle is Ts；
Ts: restore, tetra-zone of 2-2-2-2.
Said process repeats, and thus asynchronised handover changes each i.e. zone length of band chromatographic column number.
Simulation moving bed device shown in Fig. 4 particularly as follows: arrange a loop, six zone, 1-1-2-1-1-2, wherein
First band independence and gradient elution, separates three components A, B and C.
Eluent D1 in fluid reservoir D1 by infusion pump P2 pump into input bus L12, eluent D2 in fluid reservoir D2 by
Infusion pump P4 pumps into input bus L14, eluent D3 and is pumped into input bus L15, eluent by infusion pump P5 in fluid reservoir D3
D4 is pumped into input bus L16 by infusion pump 6 in fluid reservoir D4；The threeway former intercepting pipeline of L24, L23, L22 output bus goes out
Seal with plug at Kou.
Mode of operation particularly as follows:
Z1:V112, V114 and V124 open, and by eluent D1 and D2 gradient elution component A, fix and regenerate mutually, and component A flows out
Liquid stream enters fluid reservoir A；
Z2:V215 and T2 opens, and makees flowing phase, fine separation component A and B with D3；
Z3 and Z4:V313, T3 and V423 open, and component A, B are adsorbed and separate, and component A, B mixed liquor are by walking around pipeline
L21-L13 provides, and component B effluent flows into fluid reservoir B；
Z5:V516, V521 and T5 open, and with D4 elution fraction A and B, fix and regenerate mutually, an A and B mixture effluent part
Flowing into Z3 through walking around pipeline, a part is recycled to Z6；
Z6:T6 opens, component A, B mixture and component C fine separation；
Z7 and Z8:V711, T7 and V822 open, and mixture A, B, C are adsorbed and separate, and component C effluent flows into fluid reservoir
C。
Simulation moving bed device shown in Fig. 5 participates in separation, execution sequence particularly as follows: arrange Z1～Z4 totally 4 root chromatogram columns
Chromatographic isolation, each band independent operating, it is possible to carry out separating four sections of fraction A, B, C and W, or carry out gradient elution.
Eluent D1 in fluid reservoir D1 by infusion pump P2 pump into input bus L12, eluent D2 in fluid reservoir D2 by
Infusion pump P3 pumps into input bus L13, eluent D3 and is pumped into input bus L14 by infusion pump P4 in fluid reservoir D3；Respectively by
L24, L23, L22 and L21 output component A is to fluid reservoir A, component B to fluid reservoir B, component C to fluid reservoir C and component W to liquid storage
Tank W；Seal with plug at the threeway former interception tube way outlet of L24, L23, L22 output bus
Mode of operation particularly as follows:
Z1:V114, V124 open, and with eluent D1 elution fraction A, fix and regenerate mutually, and component A effluent flows into fluid reservoir A；
Z2:V213 and V223 opens, and makees flowing phase, fine separation component B with D2；
Z3:V312 and V322 opens, and makees flowing phase, fine separation component C with D3；
Z4:V411 and V421 opens, and component A of sample introduction liquid, B, C, W are adsorbed and separate, and W effluent flows into fluid reservoir B；
Simulation moving bed device shown in Fig. 6 is specially " Flos Cannabis formula " tail head of chromatographic column and is connected.
The most only consider the set-up mode of chromatograph intercolumniation circulation line, do not consider duty.8 root chromatogram columns are arranged in order
Serial number: Z1, Z2, Z3, Z4, Z5, Z6, Z7, Z8, set N root chromatogram column participate in separation process, 3≤N≤8, chromatograph during N=8
The connected mode of post is: Z1, Z3, Z5, Z7, Z8, Z6, Z4, Z2, Z1, it may be assumed that two ends Z7 and Z8 tail head is connected, Z2 Yu Z1 tail prime minister
Even, other interval chromatographic column tail head is connected, and constitutes the loop of 8 root chromatogram columns；When selecting the chromatographic column number participating in separating, this
Plant circulation line isometric, and connected mode is simple to operate, such as: be converted to as N=6 or by the connected mode of chromatographic column during N=8
During N=6, Z5 circulation line being connected in Z6 arrival end, link circuit is: Z1, Z3, Z5, Z6, Z4, Z2, Z1, it may be assumed that two ends Z5
Be connected with Z6 tail head, Z2 with Z1 tail head is connected, and other interval chromatographic column tail head is connected, and constitutes the loop of 6 root chromatogram columns；Work as N=7
Time or by when during N=8, the connected mode of chromatographic column is converted to N=7, Z6 circulation line is connected in Z7 arrival end, connects back to
Lu Wei: Z1, Z3, Z5, Z7, Z6, Z4, Z2, Z1, it may be assumed that two ends Z7 and Z6 tail head is connected, Z2 with Z1 tail head is connected, and other is spaced color
Spectrum post tail head is connected, and constitutes the loop of 7 root chromatogram columns；
Setting by this circulation line, it is possible to readily the device of the present embodiment is constituted and overlap moving bed more, such as,
During N=8, Z3 circulation line is connected in Z4 arrival end, Z6 circulation line is connected in Z5 arrival end, i.e. may make up each 4 posts of two sets
Moving bed, it (can be different flowing phase, different fixing phase, different former that two set moving bed systems can be arranged to independent operating
Feed liquid), parallel running, or series operation.
Simulation moving bed device shown in Fig. 7 is particularly as follows: " Flos Cannabis formula " tail head of chromatographic column is connected, and two 1-1-2 simulate
Moving bed loop, separation component A, B and C.
Eluent D1 in fluid reservoir D1 by infusion pump P2 pump into input bus L12, eluent D2 in fluid reservoir D2 by
Infusion pump P5 pumps into input bus L15.Seal with plug at the threeway former interception tube way outlet of L23, L22 output bus.
Mode of operation particularly as follows:
First the loop order of connection is: Z1, Z3, Z4, Z2 and Z1；
Z1:V112 and V124 opens, and with eluent D1 elution fraction A, fixes and regenerates mutually, and a component A effluent part flows into
Fluid reservoir A, a part is back to Z3 through reflux pipe L24-L16；
Z3:V316 and T3 opens, component A and B fine separation；
Z4 and Z2:V413, T4 and V223 open, and component A, B are adsorbed and separate, and component A, B mixed liquor are by walking around pipeline
L21-L13 provides, and component B effluent flows into fluid reservoir B；
Second the loop order of connection is: Z5, Z7, Z8, Z6 and Z5.
Z5:V515, V521 and T5 open, and with D2 elution fraction A and B, fix and regenerate mutually, an A and B mixture effluent part
Flowing into Z4 through walking around pipeline, a part is recycled to Z7；
Z7:T7 opens, component A, B mixture and component C fine separation；
Z8 and Z6:V811, T8 and V622 open, and in material liquid, mixture A, B, C are adsorbed and separate, and component C flows out liquid stream
Enter fluid reservoir C.
Disconnect the connecting line between 2 set simulation moving beds, may be constructed 3～7 set simulation moving beds and control system, be equipped with
Pump, pipeline, threeway and fluid reservoir, carry out 4-14 Component seperation.
Claims (9)
1. a simulation moving bed device, including M root chromatogram column, it is characterised in that 4≤M≤30, every root chromatogram column entrance and going out
Mouth connects entrance manifold and outlet manifold respectively, and entrance manifold connects following of 6 intake lines and previous root chromatogram column respectively
Endless tube road, outlet manifold connects 4 output pipes and the circulation line of current chromatographic column respectively；Every described intake line
Or output pipe connects with corresponding input bus or output bus respectively；Material liquid, eluent are total by corresponding input respectively
Line inputs the intake line of corresponding chromatographic column；Described circulation line connects previous root chromatogram column outlet manifold and current chromatographic column
Entrance manifold, makes all chromatographic columns be connected by circulation line tail head；Various column effluent in addition to circulation effluent
Corresponding output bus is exported by corresponding output pipe respectively by corresponding chromatographic column；
Material liquid, eluent are stored in corresponding fluid reservoir；The various column effluent flowed out from output bus are i.e. simulated
The system effluent of moving bed is stored in corresponding fluid reservoir；
It is respectively provided with two-port valve on every intake line of root chromatogram column, output pipe and circulation line；Described two-port valve is by electromagnetic valve
Form with check (non-return) valve, and controlled each two-port valve for being turned on and off state by PLC or single-chip computer control system；
Described chromatographic column works under the constant temperature in the range of-10 DEG C～200 DEG C；
Wherein, the chromatographic column participating in separation process in said device is N root, and 3≤N≤M, N root chromatogram column passes through circulation line
Tail head is connected, and forms loop.
A kind of simulation moving bed device the most according to claim 1, it is characterised in that by defeated to an output bus and one
Enter bus to connect, constitute and intercept pipeline.
A kind of simulation moving bed device the most according to claim 2, it is characterised in that open the current color exporting effluent
A rear root chromatogram column of the spectrum output pipe two-port valve being connected with described intercepting pipeline of post and this post with described intercepting pipeline
The intake line two-port valve being connected, constitutes reflux pipe, and arranges delivery pump on reflux pipe；
Or arranging 1 threeway and 1 delivery pump in intercepting pipeline, a mouth of described threeway is used for exporting effluent, with
Time open the output pipe two-port valve being connected with described intercepting pipeline and rear the one of this post of chromatographic column of current output effluent
The intake line two-port valve being connected with described intercepting pipeline of root chromatogram column, equally constitutes reflux pipe；
Further, above two constitutes in the mode of reflux pipe, when the reflux pipe of current chromatographic column is opened, by current chromatograph
Post circulation line is closed.
A kind of simulation moving bed device the most according to claim 2, it is characterised in that open the current color exporting effluent
Spectrum post the output pipe two-port valve being connected with described intercepting pipeline and in addition to a rear root chromatogram column of this post any one color
The intake line two-port valve being connected with described intercepting pipeline of spectrum post, constitutes and walks around pipeline；
Described walking around arranges 0～1 delivery pump in pipeline.
A kind of simulation moving bed device the most according to claim 1, it is characterised in that for same mode of operation,
In switching cycle, import, exit position are set by control system time segment, adjust the most each band of length of each function zone
Chromatographic column number.
6. according to a kind of simulation moving bed device described in any one in Claims 1 to 5, it is characterised in that described M root
The serial number that chromatographic column is arranged in order: Z1, Z2, Z3, Z4, Z5 ..., Z (n-1), Zn, Z (n+1) ..., ZM, then at described N root
In chromatographic column, the adjacent chromatographic column tail head coming two ends is connected, and other chromatographic column tail head separately is connected, chromatographic column tail prime minister
Even being described circulation line, all circulation lines are isometric；
When N is even number, the connected mode of N root chromatogram column is: Z1, Z3, Z5 ..., Z (N-3), Z (N-1), ZN, Z (N-2), Z (N-
4) ..., Z4, Z2, Z1, it may be assumed that by odd number increase direction, 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, and even number chromatographic column tail prime minister is connected to other end Z2, Z2 and Z1 tail head and is connected, and constitutes
The loop of N root chromatogram column, is connected for " Flos Cannabis formula " tail head；
When N is odd number, ZN with Z (N-1) tail head is connected, and other is identical with the situation that N is even number.
7. according to a kind of simulation moving bed device described in claim 1, it is characterised in that the simulation of N root chromatogram column is moved
Movable bed is decomposed into 2 set simulation moving bed systems, it may be assumed that L root chromatogram column tail 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 set simulation moving bed systems are independent fortune
Row mode, parallel running mode or series operation pattern.
A kind of simulation moving bed device the most according to claim 1, it is characterised in that all chromatographic columns are arranged at one
Region, all two-port valves are arranged at another one region, and chromatograph columnar region is carried out temperature control.
A kind of simulation moving bed device the most according to claim 1, it is characterised in that be equipped with on input bus filter,
Online degasser, circulation line is equipped with effusion meter, and output bus is equipped with effusion meter, solution concentration and the detector of purity.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610832972.6A CN106166402B (en) | 2016-09-19 | 2016-09-19 | A kind of moving bed imitation chromatogram separation facility |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610832972.6A CN106166402B (en) | 2016-09-19 | 2016-09-19 | A kind of moving bed imitation chromatogram separation facility |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106166402A true CN106166402A (en) | 2016-11-30 |
| CN106166402B CN106166402B (en) | 2018-06-29 |
Family
ID=57376481
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610832972.6A Active CN106166402B (en) | 2016-09-19 | 2016-09-19 | A kind of moving bed imitation chromatogram separation facility |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106166402B (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109738550A (en) * | 2019-02-25 | 2019-05-10 | 青岛众瑞智能仪器有限公司 | Continuous purification experimental provision |
| CN110665256A (en) * | 2019-10-08 | 2020-01-10 | 中国科学院过程工程研究所 | Simulated moving bed device and method for separating multicomponent dihydric alcohol |
| CN112639462A (en) * | 2018-11-16 | 2021-04-09 | 奥加诺株式会社 | Simulated moving bed mode chromatographic separation method and simulated moving bed mode chromatographic separation system |
| 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 |
| 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 |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
-
2016
- 2016-09-19 CN CN201610832972.6A patent/CN106166402B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN112639462A (en) * | 2018-11-16 | 2021-04-09 | 奥加诺株式会社 | Simulated moving bed mode chromatographic separation method and simulated moving bed mode 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 |
| CN112639462B (en) * | 2018-11-16 | 2024-05-28 | 奥加诺株式会社 | Simulated moving bed type chromatographic separation method and simulated moving bed type chromatographic separation system |
| CN109738550A (en) * | 2019-02-25 | 2019-05-10 | 青岛众瑞智能仪器有限公司 | Continuous purification experimental provision |
| 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 |
| CN110665256A (en) * | 2019-10-08 | 2020-01-10 | 中国科学院过程工程研究所 | Simulated moving bed device and method for separating multicomponent dihydric alcohol |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106166402B (en) | 2018-06-29 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106166402B (en) | A kind of moving bed imitation chromatogram separation facility | |
| JP4966449B2 (en) | Separation method using chromatographic zones of variable length | |
| CN102151418B (en) | Separation method and device for simulated moving bed | |
| CN108037233A (en) | The multidimensional liquid chromatographic separation system of full on-line checking based on same detector | |
| JP5330499B2 (en) | Gradient elution multi-column separation method | |
| CN101166564B (en) | Method and device for chromatographic purification | |
| CN102895799B (en) | The moving-bed adsorption separation method that control valve quantity reduces and equipment | |
| CN206334397U (en) | A kind of moving bed imitation chromatogram separation facility | |
| CN104056467B (en) | Five district's series connection supercritical carbon dioxide fluid simulated movable bed chromatography device and operational approach thereof | |
| CN101732890B (en) | Three-section simulated moving bed chromatography device | |
| WO2011136533A2 (en) | Chromatography apparatus and method | |
| US7618539B2 (en) | Simulated moving bed chromatography for strongly retained compounds | |
| CN207586196U (en) | The multidimensional liquid chromatographic separation system of full on-line checking based on same detector | |
| CN102123775B (en) | Simulated-moving-bed separation method and device with modulated tapped-off fluid flow | |
| CN104614458B (en) | A kind of circulation preparative high-performance liquid chromatographic instrument with multiple-way valve | |
| CN203989958U (en) | Five district's series connection simulated movable bed chromatography devices | |
| JP6758658B2 (en) | Valve manifold for pseudo-moving floor chromatography | |
| JP6013639B1 (en) | Chromatographic separation method and apparatus for separating multiple components into three or more fractions | |
| CN105617714A (en) | Asynchronous switching three-zone-belt simulation moving bed | |
| CN201618442U (en) | Three-band analogue moving bed chromatogram device | |
| CN207198107U (en) | A kind of cascade Coupled columns mass spectrometer system based on valve | |
| JPH0843372A (en) | Separation method by chromatography in simulated moving phase using correction of gap capacity caused by shortening of length | |
| CN104606921B (en) | A kind of twin columns circulation preparative high-performance liquid chromatographic instrument and the method for the preparation of separation and purification | |
| CN110025982A (en) | Multidimensional liquid chromatographic separation system based on two ten-way valves | |
| ITMI991705A1 (en) | ALTERNATE COMMUNICATION SYSTEM OF AT LEAST FOUR FLUIDS AND ITS APPLICATION IN A SEPARATION PROCEDURE IN MOBILE BED YES |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| CB03 | Change of inventor or designer information | ||
| CB03 | Change of inventor or designer information |
Inventor after: Wang Shaoyan Inventor after: Wang Jiesheng Inventor before: Wang Shaoyan Inventor before: Zhang Tianhao |
|
| GR01 | Patent grant | ||
| GR01 | Patent grant |