CN103071312A - Intermittent chromatographic separation device and method - Google Patents

Intermittent chromatographic separation device and method Download PDF

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CN103071312A
CN103071312A CN2013100457366A CN201310045736A CN103071312A CN 103071312 A CN103071312 A CN 103071312A CN 2013100457366 A CN2013100457366 A CN 2013100457366A CN 201310045736 A CN201310045736 A CN 201310045736A CN 103071312 A CN103071312 A CN 103071312A
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valve
pneumatic
chromatographic column
eluent
conveying device
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王兆光
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SHANDONG TRILLION CHROMATOGRAPHY SEPARATION TECHNOLOGY Co Ltd
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SHANDONG TRILLION CHROMATOGRAPHY SEPARATION TECHNOLOGY Co Ltd
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Abstract

The invention discloses an intermittent chromatographic separation device which comprises a separation device, a raw material conveying device, an eluent conveying device and a collection device; the raw material conveying device and the eluent conveying device are respectively connected with the input end of the separation device; and the collection device is connected with the output end of the separation device. The invention also discloses an intermittent chromatographic separation method which comprises the following process that (1) a large chromatographic circulation separation process is carried out; (2) a small chromatographic circulation separation process is carried out; and (3) an all-in all-out chromatographic separation process is carried out. According to the intermittent chromatographic separation device and the intermittent chromatographic separation method, the defects in the separation system of a traditional continuous simulation mobile bed are overcome, a novel process of the simulation mobile bed is implemented, the process is convenient to operate and works stably, all indicators are optimal, not only is the utilization rate of a separation medium improved, but also the water consumption can be reduced and the degree of impact to resin is reduced.

Description

Batch (-type) chromatographic separation device and method
Technical field
The present invention relates to a kind of chromatographic separation technology, specifically a kind of batch (-type) chromatographic separation device and method.
Background technology
The traditional analog moving bed forms closed cycle by the series connection of many pillars (being generally the 6-12 root forms) head and the tail.As shown in Figure 1, the delivered inside (pillar quantity can adopt 2 10 when above) that a delivery pump P1 carries out feed liquid is installed in the circulation line optional position; Configure FIC1 of flowmeter for detection of the internal system flow at pump discharge; In circulation line optional position installation quality flowmeter DIC1 detectable concentration bands of a spectrum situation of change; At delivery side of pump setting pressure sensor PT1, be used for the testing pump outlet pressure; 1 charging switch valve KS1 and a water inlet switch valve KS2 are installed in the import of each pillar; The outlet of each pillar is installed one and is gone out slow component switch valve KS3 and one and go out fast component switch valve KS4; The eluent inlet flow rate is Q2, by flowmeter FIC2 and intake pump P2 VFC, the slow component rate of discharge is Q4, by flowmeter FIC4 and control valve FCV4 control, the material liquid inlet flow rate is Q3, by flowmeter FIC3 and feed pump P3 VFC, detect slow component concentration by DIC4, the fast component rate of discharge is Q5, by flowmeter FIC5 and control valve FCV5 control, detect fast component concentration by DIC5, these 4 mouths will simulation moving-bedly be divided into 4 districts, and the district between eluent entrance and slow component export is called the Z1 district; Be the Z2 district between slow component outlet and the material liquid entrance; Be the Z3 district between material liquid entrance and the fast component outlet; Be the Z4 district between fast component outlet and the eluent entrance; Four mouths move to respectively the correspondence position of next pillar along the mobile phase direction in setting-up time, reach mobile phase and move with fixing adverse current mutually.
As shown in Figure 2, the traditional analog moving bed method of operation is to move according to the parameter of setting, setup parameter comprises T cycle time, circular flow Q1, flow of inlet water Q2, slow component discharge Q4, feed rate Q3, fast component discharge Q5, in system's running, 2 flow Q2, Q3 entering system enter system by pump P2, P3 sustainable supply, and 2 kinds of dischargings are respectively by the chain control of FIC4/FCV4, FIC5/FCV5, this operational mode is continuous the entering in the system of eluting water and material liquid, and slow component and fast component are discharged continuously.Material and eluting water constantly enter system in continuous separation process, and material and eluting water constantly are dispersed in the system, and actual is that back-mixing is caused in the subregion, has taken time and the space of whole piece-rate system, and the utilization rate of separating medium has reduced.
Because eluting water constantly is dispersed, be actually used in Z4 separate from the space greatly reduced, the ability of utilizing of traditional chromatographic fractionation system inner loop water reduces, reality has increased water consumption;
Because traditional chromatographic isolation tradition circulating pump is few, after the resistance accumulation through several pillars, forms larger pressure at pump discharge, causes higher pressure reduction, resin is caused in various degree impact.
Summary of the invention
For above-mentioned deficiency, the invention provides a kind of batch (-type) chromatographic separation device and method, it has not only improved the utilization rate of separating medium, and can reduce water consumption, has reduced the impact degree to resin.
The present invention solves the technical scheme that its technical problem takes:
The invention provides a kind of batch (-type) chromatographic separation device, comprise separator, raw material conveying device, eluant, eluent conveying device and gathering-device, described raw material conveying device is connected with the eluant, eluent conveying device and is connected input with separator and connects, described gathering-device is connected output and is connected with separator, it is characterized in that, described separator comprises some chromatographic columns, the import of described each chromatographic column and outlet all arrange a pressure sensor, each chromatographic column outlet arranges a circulation dehvery pump, one of them exit of described circulation dehvery pump is provided with flowmeter, one of them exit of described circulation dehvery pump is provided with mass flowmenter, and the import department of described each chromatographic column and exit arrange respectively two pneumatic on-off valves; Described raw material conveying device comprises material container and is arranged on control valve and pressure sensor on the feed pipe; Described eluant, eluent conveying device comprises the eluant, eluent container and is arranged on control valve and pressure sensor on the inlet channel; Described gathering-device comprises the two-way discharge pipe, and described each road discharge pipe is respectively arranged with flowmeter, mass flowmenter and control valve.
Further, described pneumatic on-off valve comprises charging pneumatic on-off valve, water inlet pneumatic on-off valve, intercolumniation pneumatic on-off valve, slow component discharging pneumatic on-off valve and fast component discharging pneumatic on-off valve, described charging pneumatic on-off valve and water inlet pneumatic on-off valve are arranged on the import department of each chromatographic column, described intercolumniation pneumatic on-off valve is arranged on the connecting pipe of each chromatographic column, and between chromatographic column import and export pneumatic on-off valve; Described slow component discharging pneumatic on-off valve and fast component discharging pneumatic on-off valve are arranged on the exit of each chromatographic column.
Further, described discharge pipe comprises slow component discharge pipe and fast component discharge pipe.
The present invention also provides a kind of batch (-type) chromatography separating method, it is characterized in that, comprises following process:
1) process of chromatogram systemic circulation separation: the closed pneumatic valve on closeall chromatographic column and raw material conveying device, eluant, eluent conveying device and the gathering-device connecting line, carry out the circulation of separator internal composition, this process is labeled as the A section;
2) the chromatogram partial circulating process of separating: open the fast component discharging pneumatic on-off valve that water inlet pneumatic on-off valve that Z1 district chromatographic column is connected with the eluant, eluent conveying device and chromatographic column are connected with the fast component discharge pipe, open simultaneously the intercolumniation pneumatic on-off valve in Z1 district, Z2 district and Z3 district, the fast component of execution discharging equivalent when injecting eluant, eluent, this process is labeled as the B section;
3) process of chromatogram all-in and all-out separation: carry out simultaneously and utilize eluant, eluent wash-out slow component process and input raw material to discharge equivalent fast component process,
The described eluant, eluent wash-out slow component process of utilizing is to open the slow component discharging pneumatic on-off valve that water inlet pneumatic on-off valve that Z1 district chromatographic column is connected with the eluant, eluent conveying device and chromatographic column are connected with the slow component discharge pipe, carries out the slow component of discharging equivalent when injecting eluant, eluent.This process is labeled as the C section,
It is to open the fast component discharging pneumatic on-off valve that charging pneumatic on-off valve that Z3 district chromatographic column is connected with raw material conveying device and chromatographic column are connected with the fast component discharge pipe that described input raw material is discharged equivalent fast component process, open simultaneously the intercolumniation pneumatic on-off valve in Z3 district, carry out the fast component of when injecting raw material, discharging equivalent.This process is labeled as the D section;
Wherein, before carrying out said process, need the relevant parameter of A, B, C, each section of D is arranged.
Preferably, described relevant parameter comprises setting flow Qa, Qb, Qc, the Qd of A, B, C, D section, and A, B, C, flow volume Va, the Vb of D section, Vc, Vd.
The invention has the beneficial effects as follows: the present invention has overcome the drawback in traditional continuous analog moving bed piece-rate system, a kind of simulation moving-bed new technology of implementation, and this technological operation is convenient, stable, indices reaches optimization.The present invention has not only improved the utilization rate of separating medium, and can reduce water consumption, has reduced the impact degree to resin.
Description of drawings
Fig. 1 is the structural representation of traditional analog moving bed;
Fig. 2 is the process schematic representation of traditional analog moving bed;
Fig. 3 is structural representation of the present invention;
Fig. 4 is the process schematic representation that chromatogram circulation of the present invention separates;
Fig. 5 is the process schematic representation that chromatogram of the present invention half is separated;
Fig. 6 is the full process schematic representation that separates of chromatogram of the present invention;
Fig. 7 is that the eluant, eluent of the present invention and traditional handicraft is utilized situation contrast schematic diagram;
Fig. 8 is the feed distribution situation contrast schematic diagram of the present invention and traditional handicraft;
Fig. 9 is that the Performance Ratio of the present invention and traditional handicraft is than schematic diagram;
Among the figure,
Z1-Z4 is four simulation moving-bed subregions;
KS1-KS5 is pneumatic on-off valve;
P1-P6 is circulating pump, and P7, P8 are feed pump;
SC1-SC6 is the frequency converter of circulating pump, and SC7-SC8 is the frequency converter of feed pump;
PT1-PT3 is pressure sensor;
FIC is flowmeter;
DIC1, DIC4-DIC5 are mass flowmenter;
FCV4-FCV5 is control valve.
The specific embodiment
As shown in Figure 3, a kind of batch (-type) chromatographic separation device of the present invention, it comprises separator, raw material conveying device, eluant, eluent conveying device and gathering-device, described raw material conveying device is connected with the eluant, eluent conveying device and is connected input with separator and connects, and described gathering-device is connected output and is connected with separator.Described separator comprises some chromatographic columns, the import of described each chromatographic column and outlet all arrange a pressure sensor, each chromatographic column outlet arranges a circulation dehvery pump, one of them exit of described circulation dehvery pump is provided with flowmeter, one of them exit of described circulation dehvery pump is provided with mass flowmenter, and the import department of described each chromatographic column and exit arrange respectively two pneumatic on-off valves; Described raw material conveying device comprises material container and is arranged on control valve and pressure sensor on the feed pipe; Described eluant, eluent conveying device comprises the eluant, eluent container and is arranged on control valve and pressure sensor on the inlet channel; Described gathering-device comprises the two-way discharge pipe, and described each road discharge pipe is respectively arranged with flowmeter, mass flowmenter and control valve;
Further, described pneumatic on-off valve comprises charging pneumatic on-off valve, water inlet pneumatic on-off valve, intercolumniation pneumatic on-off valve, slow component discharging pneumatic on-off valve and fast component discharging pneumatic on-off valve, described charging pneumatic on-off valve and water inlet pneumatic on-off valve are arranged on the import department of each chromatographic column, described intercolumniation pneumatic on-off valve is arranged on each chromatographic column connecting pipe, and between chromatographic column import and export pneumatic on-off valve; Described slow component discharging pneumatic on-off valve and fast component discharging pneumatic on-off valve are arranged on the exit of each chromatogram.
Further, described discharge pipe comprises slow component discharge pipe and fast component discharge pipe.
Such as Fig. 4, Fig. 5 and shown in Figure 6, the present invention also provides a kind of batch (-type) chromatography separating method, and it comprises following process:
1) process of chromatogram systemic circulation separation: the closed pneumatic valve on closeall chromatographic column and raw material conveying device, eluant, eluent conveying device and the gathering-device connecting line, carry out the circulation of separator internal composition, this process is labeled as the A section;
2) the chromatogram partial circulating process of separating: open the fast component discharging pneumatic on-off valve that water inlet pneumatic on-off valve that Z1 district chromatographic column is connected with the eluant, eluent conveying device and chromatographic column are connected with the fast component discharge pipe, open simultaneously the intercolumniation pneumatic on-off valve in Z1 district, Z2 district and Z3 district, the fast component of equivalent is discharged in execution when injecting eluant, eluent, this process is labeled as the B section;
3) process of chromatogram all-in and all-out separation: carry out simultaneously and utilize eluant, eluent wash-out slow component process and input raw material to discharge equivalent fast component process,
The described eluant, eluent wash-out slow component process of utilizing is to open the slow component discharging pneumatic on-off valve that water inlet pneumatic on-off valve that Z1 district chromatographic column is connected with the eluant, eluent conveying device and chromatographic column are connected with the slow component discharge pipe, carries out the slow component of discharging equivalent when injecting eluant, eluent.This process is labeled as the C section,
It is to open the fast component discharging pneumatic on-off valve that charging pneumatic on-off valve that Z3 district chromatographic column is connected with raw material conveying device and chromatographic column are connected with the fast component discharge pipe that described input raw material is discharged equivalent fast component process, open simultaneously the intercolumniation pneumatic on-off valve in Z3 district, carry out the fast component of when injecting raw material, discharging equivalent.This process is labeled as the D section;
Wherein, before carrying out said process, need the relevant parameter of A, B, C, each section of D is arranged; Described relevant parameter comprises setting flow Qa, Qb, Qc, the Qd of A, B, C, D section, and A, B, C, flow volume Va, the Vb of D section, Vc, Vd.
System of the present invention forms:
A kind of batch (-type) is simulation moving-bed, is made of 4-6 chromatographic column, is that the import and export of each chromatographic column is all installed a pressure sensor PT1, is used for detecting cylinder internal pressure situation of change with the explanation of 6 column systems among Fig. 4; The outlet of each chromatographic column configures one of variable-frequency circulation dehvery pump, is respectively P1, P2, P3, P4, P5, P6; Pump discharge in any one chromatographic column is installed a flowmeter FIC1, in order to control the flow of mobile phase between cylinder, regulate the FIC1 flow by control and the frequency conversion of the chain pump of FIC1, other pumps are as the auxiliary manual adjustments that adopts of the frequency of chain pump, when chain pump is higher than effective range, the illustrative system load is bigger than normal, and the frequency that needs manually to increase other pumps compensates the underpower of this pump, otherwise reduces; Pump discharge in any one chromatographic column is installed a mass flowmenter DIC1, the concentration bands of a spectrum distribution situation in the detection system; The import of each chromatographic column respectively join 2 pneumatic on-off valve KS1 KS2 be used for controlling charging and the water inlet of each cylinder; The outlet of each chromatographic column join 2 pneumatic on-off valve KS4 KS3 be used for controlling slow component and fast component discharging; 1 intercolumniation pneumatic on-off valve of every post intermediate configurations KS5 is used for controlling pipeline between the cylinder; Chromatographic system has the two-way discharging, one group is slow component discharging phase, be provided with a flowmeter FIC4, a control valve FCV4 and a mass flowmenter DIC4 at its discharge pipe, go out the extract flow on flowmeter FIC4 and this pipeline of the chain control of control valve FCV4, mass flowmenter DIC4 detects the discharging dry matter content of slow component; Another group is the fast component discharging, be provided with a flowmeter FIC5, a control valve FCV5 and a mass flowmenter DIC5 at its discharge pipe, discharging flow on flowmeter FIC5 and this pipeline of the chain control of control valve FCV5, mass flowmenter DIC5 detects the discharging dry matter content of fast component; Each cylinder is connected in series by pipe-line system, realizes automatic operating able to programme by the PLC control system.
Water inlet system is the loine pressure PT2 by control valve PCV7 control P7, guarantees the system that enters smoothly of water inlet; Feed system guarantees the system that enters smoothly of charging by the loine pressure PT3 of control PVC8 control P8.
The operating procedure of the method for the invention:
Method of the present invention adopts batch (-type) (multiple step format) method of operation, guarantees that at first pressure P T2, the PT3 of feed system moves under setting pressure, and this is the precondition of system's operation.
Batch (-type) chromatographic isolation technique is divided into 4 sections operations, and namely A, B, C, D are four sections, set 8 operational factors, and Qa, Qb, Qc, Qd represent respectively the setting flow of A, B, C, D section; Va, Vb, Vc, Vd represent respectively the accumulative total volume of every section operation, begin to switch to next step after reaching the accumulative total volume;
As shown in Figure 4, the A section is the closed circuit systemic circulation stage, and external feed and water do not enter system, namely KS1 KS2 be in closed condition, inner separation component is not discharged yet, namely KS4 KS3 all close; 6 circulating pumps of system move simultaneously, the chain frequency adjustment internal system flow by control pump of flowmeter FIC1 and pump is pressed the Qa operation, the change in concentration of DIC1 detection system inside also records concentration curve, when be recycled to the accumulative total volume when reaching Va system switch to the operation of B section.
As shown in Figure 5, the B section is the partial circulating stage, namely only goes out fast component and does not go out slow component, has got rid of the Z4 district.Outside eluting water enters system, and this moment, switch valve KS2 opened, and fast component valve KS3 opens simultaneously, and the fast component of equivalent is exhausted from system; B section circulating pump frequency is manually to set, and frequency output is identical with the A section; B section Z4 does not work, and import and export are closed, i.e. the intercolumniation KS5 valve of the entry and exit of Z4 place post connection cuts out, and other KS5 valve is still opened, and this column outlet circulating pump is stopped; The B section is controlled by 2 operational factors, and one is discharging instantaneous delivery Qb, and one is integrated flow Vb, and discharging flow Qb is by control valve FCV5 controlling run; DIC5 detects the dry concentration of discharging, and the bands of a spectrum curve map of record discharging dry; After reaching integrated flow Vb, system switches to next section C, D section.
As shown in Figure 6, the C section is for advancing eluting water wash-out slow component section, this section occurs in the Z1 district, water intaking valve KS2 opens, going out slow component switch valve KS4 opens, the outlet pump operation of Z1 district place post, enter system's eluting water with slow component equal-volume wash-out out and the discharge system, 2 parameters of C section operation, one is instantaneous delivery Qc, this flow namely is the wash-out water yield that enters system, it also is the discharge rate that the C section goes out slow component, this amount is by FIC4 and the chain control of FCV4, and one is accumulative total volume Vc, switches to the A section of next cylinder after reaching integrated flow.
The D section is discharged the stage for raw material is transfused to system's fast component by equivalent.The D section occurs in the Z3 district, the inlet valve KS1 that enters the Z3 district opens, the switch valve KS3 that goes out the Z3 district opens, the outlet pump operation of Z3 district place post, the KS5 valve between the Z3 district place post is opened, enter system's material liquid with Z3 distinguish from after the bodies such as fast component displace system, 2 parameters of D section operation, one is instantaneous delivery Qd, and it is identical with the discharge rate that goes out slow component that this flow is that the D section enters the material quantity of system, and this is measured by FIC5 and the chain control of FCV5; Another parameter is accumulative total volume Vd, namely switches to the A section of next cylinder after the turnover amount reaches integrated flow.
The operation of C section and D segment sync finishes simultaneously, when wherein one section when reaching integrated flow first, then needs to wait for the operation of the A section that together switches to next cylinder behind another section end of run before repeating.Simulation moving-bed operation is controlled by PLC, regulates control by PID.
System features of the present invention:
A, compare with traditional handicraft and can find out according to above explanation, new technology A section is to be exclusively used in the stage that circulation separates, this section is that the internal water moving system materials inside by the Z4 district circulates and separates, although the B section has the part input and output material, but still bringing into play the effect that circulation separates, and the B section promotes materials inside by outside fresh water separates, and C, D section feeding and discharging are carried out synchronously, if the flow of turnover is very large, the used time is shorter.If system scale is the same like this, compare with traditional handicraft, new technology have centrifugation A B section shared time quantum in whole separation cycle time portion of increasing charging reduce, be significantly less than the shared time of continuous feed, the new technology separative efficiency improves, good separating effect.
The purposes of eluting water that B, this batch process are intensive.Fresh eluting water is used for wash-out and separates slow component after finishing, and new technology makes fresh unboiled water by focus utilization, has reduced the contaminated chance of water, inner pool good purification; Traditional handicraft is continuously water inlet and wash-out, and fresh water constantly is dispersed in the system in promotion and elution process, and fresh water is few, and contaminated degree is large; When reaching identical clean-up effect, the water loss-rate traditional handicraft that batch (-type) needs reduces greatly.Onesize system, continous way traditional handicraft ton material water consumption is 1.2, the ton material water consumption of batch (-type) separating technology only is 0.8.The eluant, eluent of the present invention and traditional handicraft is utilized the situation contrast as shown in Figure 7, and Fig. 7 (a) is utilized the distribution map of situation for the eluant, eluent of traditional handicraft, and Fig. 7 (b) is utilized the distribution map of situation for the eluant, eluent of technique of the present invention.
C, batch (-type) charging have improved the service efficiency of medium.Because the batch (-type) charging is for concentrating feed, raw material only is distributed in the limited scope, the difficult contamination of raw material that is newly entered of the component after the separation, and namely the contaminated degree of resin reduces; Traditional handicraft is for continuing charging, and the raw material that continues to enter constantly is distributed in the system, has taken larger resin space, easily with separate after the component back-mixing, make the resin space of Z2, Z3 Disengagement zone compressed, separative efficiency descends; Batch process separates same material and can use less separation to be situated between, and the feed distribution situation of the present invention and traditional handicraft contrasts as shown in Figure 8, and Fig. 8 (a) is the feed distribution figure of traditional handicraft, and Fig. 8 (b) is the feed distribution figure of technique of the present invention.
D, batch (-type) separating technology are because interval segmentation is distinct, and same scale can be used shorter space, and general traditional separating technology adopts the 8-12 post, and batch process adopts the 4-6 post to get final product, and has greatly saved cost of investment.The Performance Ratio of the present invention and traditional handicraft more as shown in Figure 9, wherein, SMB is the traditional handicraft performance curve, SSMB is processing performance curve of the present invention.
E, because there is cumulative flow in traditional flow, flow be Q1+Q4 greater than Q3, batch process systemic circulation flow is always Q3, and is less than normal than traditional handicraft, the tangent plane linear velocity of generation is little, cylinder pressure reduction is little, flow is little to system shock in the net system switching process; When the system pressure of general traditional handicraft was 5bar, the system pressure of batch process was that 2.5bar can satisfy with interior, because the flow slight drag is little, the use power of pump is also low.
The present invention has overcome the drawback in traditional continuous analog moving bed piece-rate system, a kind of novel simulation moving-bed new technology of implementation, and this technological operation is convenient, stable, indices reaches optimization.

Claims (5)

1. batch (-type) chromatographic separation device, comprise separator, raw material conveying device, eluant, eluent conveying device and gathering-device, described raw material conveying device is connected with the eluant, eluent conveying device and is connected input with separator and connects, described gathering-device is connected output and is connected with separator, it is characterized in that, described separator comprises some chromatographic columns, the import of described each chromatographic column and outlet all arrange a pressure sensor, each chromatographic column outlet arranges a circulation dehvery pump, one of them exit of described circulation dehvery pump is provided with flowmeter, one of them exit of described circulation dehvery pump is provided with mass flowmenter, and the import department of described each chromatographic column and exit arrange respectively two pneumatic on-off valves; Described raw material conveying device comprises material container and is arranged on control valve and pressure sensor on the feed pipe; Described eluant, eluent conveying device comprises the eluant, eluent container and is arranged on control valve and pressure sensor on the inlet channel; Described gathering-device comprises the two-way discharge pipe, and described each road discharge pipe is respectively arranged with flowmeter, mass flowmenter and control valve.
2. a kind of batch (-type) chromatographic separation device according to claim 1, it is characterized in that, described pneumatic on-off valve comprises charging pneumatic on-off valve, water inlet pneumatic on-off valve, intercolumniation pneumatic on-off valve, slow component discharging pneumatic on-off valve and fast component discharging pneumatic on-off valve, described charging pneumatic on-off valve and water inlet pneumatic on-off valve are arranged on the import department of each chromatographic column, described intercolumniation pneumatic on-off valve is arranged on each chromatographic column connecting pipe, and between chromatographic column import and export pneumatic on-off valve; Described slow component discharging pneumatic on-off valve and fast component discharging pneumatic on-off valve are arranged on the exit of each chromatogram.
3. a kind of batch (-type) chromatographic separation device according to claim 1 is characterized in that, described discharge pipe comprises slow component discharge pipe and fast component discharge pipe.
4. a batch (-type) chromatography separating method is characterized in that, comprises following process:
1) process of chromatogram systemic circulation separation: the closed pneumatic valve on closeall chromatographic column and raw material conveying device, eluant, eluent conveying device and the gathering-device connecting line, carry out the circulation of separator internal composition, this process is labeled as the A section;
2) the chromatogram partial circulating process of separating: open the fast component discharging pneumatic on-off valve that water inlet pneumatic on-off valve that Z1 district chromatographic column is connected with the eluant, eluent conveying device and chromatographic column are connected with the fast component discharge pipe, open simultaneously the intercolumniation pneumatic on-off valve in Z1 district, Z2 district and Z3 district, the fast component of equivalent is discharged in execution when injecting eluant, eluent, this process is labeled as the B section;
3) process of chromatogram all-in and all-out separation: carry out simultaneously and utilize eluant, eluent wash-out slow component process and input raw material to discharge equivalent fast component process,
The described eluant, eluent wash-out slow component process of utilizing is to open the slow component discharging pneumatic on-off valve that water inlet pneumatic on-off valve that Z1 district chromatographic column is connected with the eluant, eluent conveying device and chromatographic column are connected with the slow component discharge pipe, carries out the slow component of discharging equivalent when injecting eluant, eluent.This process is labeled as the C section,
It is to open the fast component discharging pneumatic on-off valve that charging pneumatic on-off valve that Z3 district chromatographic column is connected with raw material conveying device and chromatographic column are connected with the fast component discharge pipe that described input raw material is discharged equivalent fast component process, open simultaneously the intercolumniation pneumatic on-off valve in Z3 district, carry out the fast component of when injecting raw material, discharging equivalent.This process is labeled as the D section;
Wherein, before carrying out said process, need the relevant parameter of A, B, C, each section of D is arranged.
5. a kind of batch (-type) chromatography separating method according to claim 4 is characterized in that, described relevant parameter comprises setting flow Qa, Qb, Qc, the Qd of A, B, C, D section, and A, B, C, flow volume Va, the Vb of D section, Vc, Vd.
CN2013100457366A 2013-02-05 2013-02-05 Intermittent chromatographic separation device and method Pending CN103071312A (en)

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Application publication date: 20130501