CN203989958U - Five district's series connection simulated movable bed chromatography devices - Google Patents
Five district's series connection simulated movable bed chromatography devices Download PDFInfo
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Abstract
The utility model provides a kind of five district's series connection simulated movable bed chromatography devices, that supercritical fluid chromatography device and liquid phase simulated movable bed chromatography device are integrated into the 5th district simulated movable bed chromatography device of connecting, the particularly series connection simulated movable bed chromatography device taking supercritical carbon dioxide fluid as mobile phase Wu district, its continued operation mode, barometric gradient operator scheme and modifier gradient operation mode, can realize the separation and Extraction of target component in many components; Be connected into flexibly (4+3) or (3+3) pattern, facilitate the component of optional position to separate, can realize efficient, the low consumption of many components raw material, clean scale chromatographic isolation, be specially adapted to industry preparation and separate, can bring obvious economic and social benefit.
Description
Technical field
The utility model relates to a kind of chromatogram arrangement, particularly a kind of five district's series connection simulated movable bed chromatography devices.
Background technology
Along with the research and development of the development of preparative liquid chromatography technology and a large amount of active materials, and the demand of the purifies and separates of newtype drug, efficient, large batch, the separating and purifying technology of green energy conservation more and more receive publicity.Laboratory adopts preparative liquid chromatography to separate and prepare pure material on a small scale, conventionally can only be to meet the needs that carry out biological activity test, toxicity research and clinical experimental study.At present, prepare in industry although SMBC (SMB) has appeared at medicine,, the use of organic solvent particularly poisonous organic solvent make it still have in some applications larger limitation.
For solve the fixing phase utilization rate of preparative liquid chromatography low, prepare the shortcomings such as discontinuous, separation costs is high, people will combine with Preparative Liquid Chromatography with the simulation moving-bed design philosophy of large-scale chromatography of field of food successful Application in petrochemical industry, invented possess that fixing phase utilization rate is high, the liquid phase SMBC of the advantage such as continued operation, separation costs are low, for example: patent 200510049524.0,200520101310.9 etc. discloses a kind of simulated moving bed chromatography system of three subregion open loop types, for separating of two-component mixture; Patent 200710022904.4,201110253360.9,201210037280.4 etc. discloses a kind of closed-loop simulation mobile bed chromatic system of four subregions, for separating of the mixed thing of two components, adopt four subregion closed loop modes, part mobile phase can direct reuse, reduce mobile phase use amount, cost-saving.The described SMBC technology of these inventions combines the advantage of traditional liquid chromatogram high purity separation and moving bed rectifying carrier high usage well above, in the chromatographic isolation preparation of Continuous Flow, has obtained good effect.And obtaining successful Application aspect the extensive fractionation of chiral drug.Liquid phase SMBC is 20 times of preparative liquid chromatography intermittently in the production efficiency based on the fixing phase of unit.
But, as liquid phase SMBC technology, still need to consume a large amount of organic solvents, consume 439 liters of organic solvent mobile phases if produce per kilogram product, mean and produce solvent cost that one ton of single enantiomer medicine consumes up to 1,000,000 yuans, also can bring the environmental problem can not be ignored simultaneously.Although existing supercritical fluid chromatography, liquid phase SMBC are widely used at the separation field of medicine, but how to develop an analogy prior art more efficiently, more low consumption, more clean, safer preparing chromatograph in industry new technology, the production cost that further reduces medicine or other active material, is still industry and endeavours the focus of research.
Supercritical fluid chromatography is nontoxic owing to using, not easy to blast, stable chemical nature, environmental friendliness, cheaply the supercritical carbon dioxide fluid that is easy to get is as mobile phase, environmental protection, just can make mobile phase be separated completely with sample as long as reduce pressure or rising temperature, the evaporation that does not relate to a large amount of organic solvents is reclaimed, both cost-saving, significantly reduce again the pollution to environment and the murder by poisoning to operating personnel.The problem such as can effectively solve preparative liquid chromatography or the consumption of SMBC mobile phase is large, seriously polluted, solvent recovery is complicated, is particularly suitable for the separation application of thermal sensitivity active material.Patent 200520101310.9 and patent 200510049491.X disclose respectively the supercritical fluid simulated movable bed chromatography device of a kind of three subregions and four subregions, use for reference liquid phase three subregions and four zoning simulated movable bed principles, adopt supercritical fluid as mobile phase for separating of two-component mixture, avoid the use of a large amount of organic solvents, there is the feature of environmental protection.Compared with common preparative supercritical fluid chromatography, fixing phase utilization rate is high, preparation can be continuous, and a kind of branch technique of preparing as liquid phase is showing the advantage attracting people's attention aspect the separation of chiral drug and preparation.
But, the simulation moving-bed design of supercritical fluid of current three subregions and four subregions, only can separate two-component mixture (being divided into two), for complicated multicomponent system, can only obtain target compound by secondary separation, the object to multicomponent system obtain certain limitation.
Summary of the invention
The purpose of this utility model; be to provide a kind of five district's series connection simulated movable bed chromatography devices; that supercritical fluid chromatography device and liquid phase simulated movable bed chromatography device are integrated into the 5th district simulated movable bed chromatography device of connecting; the particularly series connection simulated movable bed chromatography device taking supercritical carbon dioxide fluid as mobile phase Wu district; can realize efficient, the low consumption of many components raw material, clean scale chromatographic isolation, be specially adapted to industry preparation and separate.
The utility model is achieved in that described five district's series connection simulated movable bed chromatography devices, and it comprises SMBC, and described SMBC You Wu district is composed in series, and every district at least establishes a chromatographic column; The port of export by last chromatographic column is connected by open-close type valve successively with the entrance point of a rear chromatographic column, and the port of export of last chromatographic column is connected with the entrance point of first chromatographic column; The entrance point of every chromatographic column is connected with mobile phase entrance pipe (17), (18), injection port pipeline (16), branch road stream transfer conduit (19) by open-close type valve separately respectively; The port of export of every chromatographic column is connected with extract pipeline (21), raffinate pipeline (20), branch road stream transfer conduit (19) by open-close type valve separately respectively; The port of export of extract pipeline (21), the port of export of raffinate pipeline (20) connect respectively heated constant temperature groove (26), cyclone separator S1, S2, recycling can (30); The inner modifier of the mobile phase that mobile phase wet tank (1) is inner and modifier storage tank (5) accesses respectively mobile phase entrance pipe (17), (18) after constant flow pump, and the inner sample introduction liquid of material liquid tank (6) accesses injection port pipeline (16) after feed liquid constant flow pump (10).
SMBC You Wu described in the utility model district is composed in series, and Dang Ge district all only configures a chromatographic column, and five chromatographic columns are Z1, Z2, Z3, Z4, Z5, by the port of export of first chromatographic column successively through open-close type valve Vh1, back pressure regulator VPZ1 is connected with the entrance point of second pillar, by the port of export of second chromatographic column successively through open-close type valve Vh2, back pressure regulator VPZ2 is connected with the entrance point of the 3rd pillar, by the port of export of the 3rd chromatographic column successively through open-close type valve Vh3, back pressure regulator VPZ3 is connected with the entrance point of the 4th pillar, by the port of export of the 4th chromatographic column successively through open-close type valve Vh4, back pressure regulator VPZ4 is connected with the entrance point of the 5th pillar, by the port of export of the 5th chromatographic column successively through open-close type valve Vh5, back pressure regulator VPZ5 is connected with the entrance point of first chromatographic column, the port of export of every chromatographic column is connected with one end of branch road stream transfer conduit (19) by Ve1, Ve2, Ve3, Ve4, Ve5 open-close type valve, the port of export of every chromatographic column is connected with extract pipeline (21) by Vf1, Vf2, Vf3, Vf4, Vf5 open-close type valve respectively, and the outlet of every pillar is connected with raffinate pipeline (20) by Vg1, Vg2, Vg3, Vg4, Vg5 open-close type valve respectively, the entrance point of every chromatographic column Z1, Z2, Z3, Z4, Z5 is connected with the other end of branch road stream transfer conduit (19) by open-close type valve Va1, Va2, Va3, Va4, Va5 separately respectively, and branch road stream transfer conduit (19) is provided with branch road transmission pump (22), back pressure regulator VPZ6, open-close type valve Vb1, Vb2, Vb3, Vb4, Vb5 are connected with injection port pipeline (16), open-close type valve Vc1, Vc2, Vc3, Vc4, Vc5 are connected with mobile phase entrance pipe (17), and open-close type valve Vd1, Vd2, Vd3, Vd4, Vd5 are connected with mobile phase entrance pipe (18), be connected to raffinate pipeline (20) upper, be connected to successively mass flowmenter F4, flow control valve VR4, back pressure regulating valve VPZ7, heated constant temperature groove (26), upper at extract pipeline (21), be connected to successively mass flowmenter F5, flow control valve VR5, back pressure regulating valve VPZ8, heated constant temperature groove (26), two heated constant temperature grooves (26) are connected with cyclone separator S1, S2 entrance respectively, the outlet at bottom of cyclone separator S1, S2 connects recycling can (30) by open-close type valve Vi1, Vi2 separately respectively, and the top outlet of cyclone separator S1, S2 connects back pressure regulating valve VPZ9, active carbon filter (27), cooler (29), mobile phase wet tank (1) after merging by check valve or open-close type valve respectively, after being connected to successively constant pressure pump (2), surge tank (3), heating thermostat (4) on the export pipeline of mobile phase wet tank (1), be connected with mobile phase carbon dioxide pipeline (9), mobile phase carbon dioxide pipeline (9) is connected with mobile phase carbon dioxide constant flow pump (11), (12), (14) arrival end by open-close type valve VK6, VK7, VK8 respectively, the modifier being provided by modifier tank (5) is connected with modifier constant flow pump (13), (15) arrival end respectively through modifier pipeline (8) by open-close type valve VK4, the port of export of mobile phase carbon dioxide constant flow pump (14), the port of export of modifier constant flow pump (15) are through pipeline be linked in sequence mixing chamber M1, flow control valve VR1, mass flowmenter F1 and mobile phase entrance pipe (18), the port of export of mobile phase carbon dioxide constant flow pump (12), the port of export of modifier constant flow pump (13) are through pipeline be linked in sequence mixing chamber M2, flow control valve VR2, mass flowmenter F2 and mobile phase entrance pipe (17), the feed liquid providing from material liquid tank (6) is connected with feed liquid constant flow pump (10) entrance with feed liquid pipeline (7) by open-close type valve VK5, and the port of export of mobile phase carbon dioxide constant flow pump (11), the port of export of feed liquid constant flow pump (10) are through pipeline be linked in sequence mixing chamber M3, flow control valve VR3, mass flowmenter F3 and injection port pipeline (16), mobile phase entrance pipe (18) is connected with chromatographic column Z1, Z2, Z3, Z4, Z5 arrival end through open-close type valve Vd1, Vd2, Vd3, Vd4, Vd5 respectively, mobile phase entrance pipe (17) is connected with chromatographic column Z1, Z2, Z3, Z4, Z5 arrival end through open-close type valve Vc1, Vc2, Vc3, Vc4, Vc5 respectively, injection port pipeline (16) is connected with chromatographic column Z1, Z2, Z3, Z4, Z5 arrival end through open-close type valve Vb1, Vb2, Vb3, Vb4 Vb5 respectively.
Five district's series connection simulated movable bed chromatography devices described in the utility model are located in system insulating box.
The beneficial effects of the utility model are:
The continued operation mode of ①Wu district series connection simulated movable bed chromatography device, can solve the low efficiency problem that existing supercritical fluid chromatography brings due to the shortcoming of intermittently operated;
②Wu district series connection simulated movable bed chromatography device, owing to adopting Co 2 supercritical fluid to replace organic solvent as mobile phase, can solve liquid phase SMBC due to the organic solvent high flow rate, the high pollution problem that adopt organic solvent to bring as mobile phase;
③Wu district series connection simulated movable bed chromatography device, can implement gradient operation mode easily, and especially barometric gradient operator scheme and modifier gradient operation mode significantly improves the separative efficiency of this device;
④Wu district series connection simulated movable bed chromatography device, distinguishing feature is, can realize the separation and Extraction of target component in many components, significantly improves the separation advantage of device;
⑤Wu district series connection simulated movable bed chromatography device, can be connected into (4+3) or (3+3) pattern flexibly, facilitates the component of optional position to separate, very suitable plant-scale compound separation application.
The utility model is by the five-zoning simulated movable bed design of supercritical fluid, can reach from multicomponent system optionally, Continuous Flow ground, first separation obtains wherein a kind of target compound, greatly improved separative efficiency, and saved separation costs.Adopt the CO of supercriticality
2fluid, as mobile phase, has been avoided the use of a large amount of organic solvents, becomes a kind of green separation technique, does not produce environmental pollution or brings food-safety problem, and the utility model, for the separation application of compound, can bring obvious economic and social benefit.
Brief description of the drawings
Fig. 1 is five district's series connection simulated movable bed chromatography device schematic diagrames described in the utility model.
Fig. 2 is five district's series connection simulated movable bed chromatography device (4+3) pattern reduced graphs described in the utility model.
Fig. 2 (A) is current period (4+3) pattern reduced graph.
Fig. 2 (B) is next cycle (4+3) pattern reduced graph.
Fig. 3 is five district's series connection simulated movable bed chromatography device (3+3) pattern reduced graphs described in the utility model.
Fig. 3 (A) is current period (3+3) pattern reduced graph.
Fig. 3 (B) is next cycle (3+3) pattern reduced graph.
In figure: 1. mobile phase wet tank, 2. constant pressure pump, 3. surge tank, 4. heating thermostat, 5. modifier tank, 6. material liquid tank, 7. feed liquid pipeline, 8. modifier pipeline, 9. mobile phase carbon dioxide pipeline, 10. feed liquid constant flow pump, 11. carbon dioxide constant flow pumps, 12. carbon dioxide constant flow pumps, 13. modifier constant flow pumps, 14. carbon dioxide constant flow pumps, 15. modifier constant flow pumps, 16. injection port pipelines, 17. mobile phase entrance pipes, 18. mobile phase entrance pipes, 19. branch road stream transfer conduit, 20. raffinate pipelines, 21. extract pipelines, 22. branch road transmission pumps, 24. system insulating boxs, 25. computer control systems, 26. heated constant temperature grooves, 27. active carbon filters, 28. carbon dioxide liquid storage steel cylinders, 29. coolers, 30. recycling cans.
Detailed description of the invention
Five district's series connection simulated movable bed chromatography devices described in the utility model, as shown in Figure 1, Figure 2, shown in Fig. 2 (A), Fig. 2 (B), Fig. 3, Fig. 3 (A), Fig. 3 (B), it comprises SMBC, and described SMBC adopts supercritical carbon dioxide fluid as mobile phase; Described SMBC You Wu district is composed in series, and every district at least establishes a chromatographic column; The port of export by last chromatographic column is connected by open-close type valve successively with the entrance point of a rear chromatographic column, and the port of export of last chromatographic column is connected with the entrance point of first chromatographic column; The entrance point of every chromatographic column is connected with mobile phase entrance pipe (17), (18), injection port pipeline (16), branch road stream transfer conduit (19) by open-close type valve separately respectively; The port of export of every chromatographic column is connected (19) by open-close type valve separately with extract pipeline (21), raffinate pipeline (20), branch road stream transfer conduit respectively; The port of export of extract pipeline (21), the port of export of raffinate pipeline (20) connect respectively heated constant temperature groove (26), cyclone separator S1, S2, recycling can (30); The inner modifier of the mobile phase that mobile phase wet tank (1) is inner and modifier storage tank (5) accesses respectively mobile phase entrance pipe (17), (18) after constant flow pump, and the inner sample introduction liquid of material liquid tank (6) accesses injection port pipeline (16) after feed liquid constant flow pump (10).
SMBC You Wu described in the utility model district is composed in series, and Dang Ge district all only configures a chromatographic column, and five chromatographic columns are Z1, Z2, Z3, Z4, Z5, by the port of export of first chromatographic column successively through open-close type valve Vh1, back pressure regulator VPZ1 is connected with the entrance point of second pillar, by the port of export of second chromatographic column successively through open-close type valve Vh2, back pressure regulator VPZ2 is connected with the entrance point of the 3rd pillar, by the port of export of the 3rd chromatographic column successively through open-close type valve Vh3, back pressure regulator VPZ3 is connected with the entrance point of the 4th pillar, by the port of export of the 4th chromatographic column successively through open-close type valve Vh4, back pressure regulator VPZ4 is connected with the entrance point of the 5th pillar, by the port of export of the 5th chromatographic column successively through open-close type valve Vh5, back pressure regulator VPZ5 is connected with the entrance point of first chromatographic column, the port of export of every chromatographic column is connected with one end of branch road stream transfer conduit (19) by Ve1, Ve2, Ve3, Ve4, Ve5 open-close type valve, the port of export of every chromatographic column is connected with extract pipeline (21) by Vf1, Vf2, Vf3, Vf4, Vf5 open-close type valve respectively, and the outlet of every pillar is connected with raffinate pipeline (20) by Vg1, Vg2, Vg3, Vg4, Vg5 open-close type valve respectively, the entrance point of every chromatographic column Z1, Z2, Z3, Z4, Z5 is connected with the other end of branch road stream transfer conduit (19) by open-close type valve Va1, Va2, Va3, Va4, Va5 separately respectively, and branch road stream transfer conduit (19) is provided with branch road transmission pump (22), back pressure regulator VPZ6, open-close type valve Vb1, Vb2, Vb3, Vb4, Vb5 are connected with injection port pipeline (16), open-close type valve Vc1, Vc2, Vc3, Vc4, Vc5 are connected with mobile phase entrance pipe (17), and open-close type valve Vd1, Vd2, Vd3, Vd4, Vd5 are connected with mobile phase entrance pipe (18), be connected to raffinate pipeline (20) upper, be connected to successively mass flowmenter F4, flow control valve VR4, back pressure regulating valve VPZ7, heated constant temperature groove (26), upper at extract pipeline (21), be connected to successively mass flowmenter F5, flow control valve VR5, back pressure regulating valve VPZ8, heated constant temperature groove (26), two heated constant temperature grooves (26) are connected with cyclone separator S1, S2 entrance respectively, the outlet at bottom of cyclone separator S1, S2 connects recycling can (30) by open-close type valve Vi1, Vi2 separately respectively, and the top outlet of cyclone separator S1, S2 connects back pressure regulating valve VPZ9, active carbon filter (27), cooler (29), mobile phase wet tank (1) after merging by check valve or open-close type valve respectively, after being connected to successively constant pressure pump (2), surge tank (3), heating thermostat (4) on the export pipeline of mobile phase wet tank (1), be connected with mobile phase carbon dioxide pipeline (9), mobile phase carbon dioxide pipeline (9) is connected with mobile phase carbon dioxide constant flow pump (11), (12), (14) arrival end by open-close type valve VK6, VK7, VK8 respectively, the modifier being provided by modifier tank (5) is connected with modifier constant flow pump (13), (15) arrival end respectively through modifier pipeline (8) by open-close type valve VK4, the port of export of mobile phase carbon dioxide constant flow pump (14), the port of export of modifier constant flow pump (15) are through pipeline be linked in sequence mixing chamber M1, flow control valve VR1, mass flowmenter F1 and mobile phase entrance pipe (18), the port of export of mobile phase carbon dioxide constant flow pump (12), the port of export of modifier constant flow pump (13) are through pipeline be linked in sequence mixing chamber M2, flow control valve VR2, mass flowmenter F2 and mobile phase entrance pipe (17), the feed liquid providing from material liquid tank (6) is connected with feed liquid constant flow pump (10) entrance with feed liquid pipeline (7) by open-close type valve VK5, and the port of export of mobile phase carbon dioxide constant flow pump (11), the port of export of feed liquid constant flow pump (10) are through pipeline be linked in sequence mixing chamber M3, flow control valve VR3, mass flowmenter F3 and injection port pipeline (16), mobile phase entrance pipe (18) is connected with chromatographic column Z1, Z2, Z3, Z4, Z5 arrival end through open-close type valve Vd1, Vd2, Vd3, Vd4, Vd5 respectively, mobile phase entrance pipe (17) is connected with chromatographic column Z1, Z2, Z3, Z4, Z5 arrival end through open-close type valve Vc1, Vc2, Vc3, Vc4, Vc5 respectively, injection port pipeline (16) is connected with chromatographic column Z1, Z2, Z3, Z4, Z5 arrival end through open-close type valve Vb1, Vb2, Vb3, Vb4 Vb5 respectively.
The simulated movable bed chromatography device of 5th district series connection described in the utility model is located in system insulating box (24).In Fig. 1, also indicate computer control system (25), carbon dioxide liquid storage steel cylinder (28), recycling can (30).
The method of operating of five district's series connection simulated movable bed chromatography devices described in the utility model: be that the order connecting successively according to chromatographic column flows to same direction at the fluid of all chromatographic column inside, along the mobile direction of fluid, set gradually mobile phase entry position by the on off state of by-pass valve control, injection port position, extract a mouthful position, carry Yu Kou position, the position, gateway of branch road, all chromatographic columns are divided into Wu Ge district, each district has a chromatographic column at least, after some cycles, by changing the on off state of valve, make mobile phase entry position, extract a mouthful position, injection port position, carry Yu Kou position, pass to next chromatographic column along the mobile direction of fluid respectively position, branch road gateway, also pass to next chromatographic column thereupon in same Wu Ge district, thereby the filler forming in mobile phase and chromatographic column moves round about.
As shown in Figure 1, above-mentioned Wu Ge district, please note the form (being white valve in Fig. 1) of valve open, the chromatographic column being positioned between mobile phase flow channel tube (18) entry position (being open-close type valve Vd1) and injection port position (being open-close type valve Vb2) belongs to subregion I, the chromatographic column being positioned between injection port position (being open-close type valve Vb2) and branch road stream mouth position (being open-close type valve Ve2) belongs to subregion II, the chromatographic column that is positioned at branch road stream mouth position (being open-close type valve Ve2) and carry between Yu Kou position (being open-close type valve Vf3) belongs to subregion III, be positioned at the chromatographic column that mobile phase flow channel tube (17) entry position (being open-close type valve Vc4) and branch road go out between stream mouth position (being open-close type valve Va5) and belong to subregion IV, the chromatographic column that is positioned at position, branch road gateway (being open-close type valve Va5) and carry between Yu Kou position (being open-close type valve Vg5) belongs to subregion V.
In Fig. 1, the situation that the on off state of all open-close type valves that five chromatographic column Z1, Z2, Z3, Z4, Z5 connect is controlled according to the external world is different and different, sample introduction district, branch road stream district also can arrange according to the required position that obtains component, mobile phase He Si district of I district mobile phase can change its polarity size according to component attribute, and the chromatographic column outlet that extract, raffinate can be positioned at respectively III district, V district from each cycle obtains; The flow, stream pressure P 1, P2, P3, P4, P5, temperature T 1, T2, T3, T4, T5, backpressure data that computer control system (25) gathers all mass flowmenter F1, F2, F3, F4, F5 implements to control flow, stream pressure, temperature, the back pressure regulating valve of all pumps, calculated gauge tap valve and obtained with suitable switching cycle break-make the separation of required component by digital-to-analogue.
In said apparatus, the on off state of all open-close type valves that are connected with five chromatographic column Z1, Z2, Z3, Z4, Z5 has five kinds of combinations, according to break-make, the switching cycle of the component gauge tap formula valve that will extract, and switches and moves in circles according to order, when injection port pattern is located between Z1 is connected with Z2, prop up way outlet and be located at Z2, between Z3 connects, SMBC (SMB) Wei Wu district series connection (4+3) form, when injection port is located between Z2 is connected with Z3, prop up way outlet and be located at Z1, between Z2 connects, SMBC (SMB) Wei Wu district series connection (3+3) form, select pattern according to the target components position that will separate, and switch open-close type valve state separately, before each district chromatographic column, open-close type valve state after chromatographic column is all by computer control system (25) operation operation, and gather all mass flows and count, the flow of control pump and the back pressure regulator of each stream, system insulating box (24) is the operating temperature of five filled columns, also by computer control.
The sample introduction of the utility model series connection Wu Ge district entrance is different from branch road stream position form, retrievable component difference.
Form one, as shown in Fig. 2, Fig. 2 (A), Fig. 2 (B), in sample, there are A, B, tri-kinds of components of C, chromatographic column between mobile phase entry position and injection port position belongs to subregion I, and (in figure, de1, de2 are mobile phase, and F is sample introduction, R1 is extract, R2 is raffinate), Main Function is the complete wash-out of realizing A, B component, to ensure the rate of recovery of B component; Chromatographic column between position, Yu Zhi crossing, injection port position belongs to subregion II, and the chromatographic column in II district is mainly adsorbed C component completely, to ensure can not be brought into branch road; The chromatographic column effect of subregion III is the B component (to ensure the rate of recovery of B) at the end of complete elution chromatography post for the previous period in each cycle, the A, the B component (to ensure B purity) that before complete adsorption chromatography post of back segment time, flow into; The effect of IV district chromatographic column is complete wash-out A component, (to ensure the purity of B); V district chromatographic column Main Function is the B component (to ensure the rate of recovery of B) flowing into before complete adsorption column.
Form two, as shown in Fig. 3, Fig. 3 (A), Fig. 3 (B), in sample, there are A, B, tri-kinds of components of C, (in figure, de1, de2 are mobile phase, F is sample introduction, and R1 is extract, and R2 is raffinate), chromatographic column between mobile phase entry position and branch road exit position belongs to subregion I, and Main Function is wash-out B, C component (to ensure the purity of B component); Between branch road exit position and injection port position, belong to subregion II, the main wash-out A component completely of II district chromatographic column, to ensure can not be brought into branch road; The chromatographic column effect of subregion III is the C component (to ensure the rate of recovery of B) at the end of complete elution chromatography post for the previous period in each cycle, the B, the C component (to ensure the rate of recovery of B) that before complete adsorption chromatography post of back segment time, flow into; The complete wash-out B of the chromatographic column effect component of subregion IV, (to ensure the rate of recovery of B); The chromatographic column Main Function of subregion V is the C component (to ensure the rate of recovery of B) flowing into before complete adsorption column.
Above-mentioned mobile phase adopts temperature, pressure to exceed the supercritical fluid of supercritical temperature, critical pressure, also can adopt subcritical fluids.
The utility model implements to separate the concrete application of polyenoic acid taking supercritical carbon dioxide fluid as mobile phase, taking C18 filler as chromatographic column, existing that brief description of the process is as follows:
As shown in Figure 1, in mobile phase wet tank (1), temperature, pressure is (T1, P1) liquid carbon dioxide, enter surge tank (3) through constant pressure pump (2) pressurization, becoming pressure is (T2, P2) liquid carbon dioxide, heating up into temperature, pressure through heating thermostat (4) is again (T3, P3) after Co 2 supercritical fluid, this supercritical carbon dioxide fluid is divided into three tunnels by mobile phase carbon dioxide pipeline (9) after pressure-reducing valve Vj2 reduces pressure pressure P 4: first via supercritical carbon dioxide fluid is connected (being mobile phase de1) with carbon dioxide constant flow pump (14) by open-close type valve VK8, and mix through mixing chamber M1 with the modifier of modifier constant flow pump (15) ratio input, mass flowmenter F1, after flow control valve VR1, inject the chromatographic column entrance of subregion I position by mobile phase entrance pipe (18) connecting valve formula valve Vd1, the second road supercritical carbon dioxide fluid is connected (being mobile phase de2) with carbon dioxide constant flow pump (12) by open-close type valve VK7, and with the modifier of modifier constant flow pump (13) ratio input through mixing chamber M2 mixes, after mass flowmenter F2, flow control valve VR2, by the chromatographic column entrance of mobile phase entrance pipe (17) connecting valve formula valve VC4 injection subregion IV position, Third Road supercritical carbon dioxide fluid is connected with carbon dioxide constant flow pump (11) by open-close type valve VK6, the polyenoic acid solution of carbon dioxide constant flow pump (11) ratio output and feed liquid constant flow pump (10) input through mixing chamber M3 mix, after mass flowmenter F3, flow control valve VR3, by the chromatographic column entrance of injection port pipeline (16) connecting valve formula valve Vb2 injection subregion II position, subregion III is extracted mouth and is connected extract pipeline (21) through open-close type valve Vf3, the supercritical fluid of this pipeline is through the flow measuring and controlling assembly adjust flux of mass flowmenter F5 and flow control valve VR5 formation, flow through after back pressure regulator VPZ8, and after heated constant temperature groove (26) heats up, entering temperature, pressure is (T4, P4) cyclone separator S2, due to intensification and the acting in conjunction of step-down, the gasification of supercritical carbon dioxide fluid moment, and because modifier solution is often much higher than the boiling point of carbon dioxide with the boiling point of solute, therefore the modifier solution of enrichment object component will be separated out with the form of micro-drop (or crystallite), then realizing gas-liquid two-phase by the effect of cyclone separator S2 separates, obtain the modifier solution of object component in the bottom of cyclone separator S2, what flow out from the top outlet of cyclone separator S2 is the carbon dioxide of only carrying micro-modifier secretly, subregion V is carried remaining mouthful and is connected raffinate pipeline (20) through open-close type valve Vg5, the supercritical fluid of this pipeline is after the Flow-rate adjustment of mass flowmenter F4 and flow control valve VR4 formation, flow through after back pressure regulator VPZ7, and after heated constant temperature groove 26 heats up, entering temperature, pressure is (T4, P4) cyclone separator S1, through similar step, realizes the modifier solution of other component of enrichment and separating of carbon dioxide, exporting from the top of cyclone separator S1, S2 the temperature, pressure converging after check valve VZ1, VZ2 is (T4, P4) carbon dioxide, the step-down after back pressure regulator VPZ9 of flowing through becomes the carbon dioxide that temperature, pressure is (P5), after active carbon filter (27) adsorption cleaning and cooler (29) cooling, becoming temperature, pressure is (T1, P1) liquid carbon dioxide, enters the liquid storage tank of mobile phase (1) and recycles.The operating pressure P4 of above-mentioned cyclone separator S1, S2 is unified to control by the back pressure regulator VPZ9 in downstream.The outlet at bottom of cyclone separator S1, S2 connects recycling can (30) by gauge tap formula valves Vi1, Vi2 respectively, then form alternation switch state with open-close type valve Vi3, Vi4, connect respectively again non-pressure vessel, guarantee cyclone separator S1, S2 internal pressure temperature in the discharge process of product and modifier.Supplementary when CO 2 fluid in carbon dioxide liquid storage steel cylinder (28) causes for special pearl operating modes such as this device drivings, cyclone separator discharging, active carbon filter, chromatographic column replacing quantity not sufficient that this installs inner carbon dioxide.
Five districts series connection simulated movable bed chromatography devices (SMB) described in the utility model are not limited in above-mentioned each subregion and have all only configured the form of implementation of 1 chromatographic column, and each subregion is the chromatographic column of configurable two also, and the annexation of device also can expand to 6th district.The demand and the number that separate according to object, by being divided into the 5th district SMB(4+3 that connects with the Switch State Combination in Power Systems of the direct-connected all open-close type valves of chromatographic column) and 5th district series connection SMB(3+3) pattern, also can expand six districts' series connection SMB(4+1+3) and the 6th district SMB(3+3+1 that connects) pattern.Above-described five district's series connection simulated movable bed chromatography devices, pass through computer control system (25) control combination with the state of the direct-connected all open-close type valves of chromatographic column, by suitable switching cycle, switch successively and make mobile phase entry position, extract mouthful position, an injection port position, carry Yu Kou position and pass and move in circles to next chromatographic column along the mobile direction of fluid respectively, just energy flexible combination is to meet separation requirement.
Fig. 2 is the SMB(4+3 of above-mentioned five subregion I, II, III, IV, V series connection) pattern.Illustrate respectively Shi five districts series connection simulated movable bed chromatography devices, in two adjacent valve switching cycles, mobile phase de1, de2 entry position, extract mouthful position, an injection port F position, carry the situation of movement schematic diagram of Yu Kou position, mobile phase exit position; Fig. 2 (A) is current period mobile phase de1, de2 entrance, extracts mouth, injection port, carries the desired location of remaining mouthful; Fig. 2 (B) is next cycle mobile phase de1, de2 entrance, extracts mouth, injection port, carries the desired location of remaining mouthful.
Fig. 3 is the SMB(3+3 of above-mentioned five subregion I, II, III, IV, V series connection) pattern.Illustrate respectively Shi five districts series connection simulated movable bed chromatography devices, in two adjacent valve switching cycles, mobile phase de1, de2 entry position, extract mouthful position, an injection port position, carry the situation of movement schematic diagram of Yu Kou position, mobile phase exit position; Fig. 3 (A) is the desired location of current period mobile phase de1, de2 entrance, extract mouth, injection port, raffinate mouth; Fig. 3 (B) is next cycle mobile phase de1, de2 entrance, extracts mouth, injection port, carries the desired location of remaining mouthful.
The utility model proposes Wu district series connection simulated movable bed chromatography device, be described by embodiment, person skilled obviously can change device as herein described or suitably change and combination in content of the present invention, spirit and scope, realizes the utility model technology.Special needs to be pointed out is, all similar replacements and change are predictable for a person skilled in the art, and they all can be believed to comprise in the utility model scope and content.
Claims (3)
1.Wu district series connection simulated movable bed chromatography device, it comprises SMBC, it is characterized in that: described SMBC You Wu district is composed in series, and every district at least establishes a chromatographic column; The port of export by last chromatographic column is connected by open-close type valve successively with the entrance point of a rear chromatographic column, and the port of export of last chromatographic column is connected with the entrance point of first chromatographic column; The entrance point of every chromatographic column is connected with mobile phase entrance pipe (17), (18), injection port pipeline (16), branch road stream transfer conduit (19) by open-close type valve separately respectively; The port of export of every chromatographic column is connected with extract pipeline (21), raffinate pipeline (20), branch road stream transfer conduit (19) by open-close type valve separately respectively; The port of export of extract pipeline (21), the port of export of raffinate pipeline (20) connect respectively heated constant temperature groove (26), cyclone separator S1, S2, recycling can (30); The inner modifier of the mobile phase that mobile phase wet tank (1) is inner and modifier storage tank (5) accesses respectively mobile phase entrance pipe (17), (18) after constant flow pump, and the inner sample introduction liquid of material liquid tank (6) accesses injection port pipeline (16) after feed liquid constant flow pump (10).
2. five districts series connection simulated movable bed chromatography devices according to claim 1, is characterized in that: described SMBC You Wu district is composed in series, and Dang Ge district all only configures a chromatographic column, and five chromatographic columns are Z1, Z2, Z3, Z4, Z5, by the port of export of first chromatographic column successively through open-close type valve Vh1, back pressure regulator VPZ1 is connected with the entrance point of second pillar, by the port of export of second chromatographic column successively through open-close type valve Vh2, back pressure regulator VPZ2 is connected with the entrance point of the 3rd pillar, by the port of export of the 3rd chromatographic column successively through open-close type valve Vh3, back pressure regulator VPZ3 is connected with the entrance point of the 4th pillar, by the port of export of the 4th chromatographic column successively through open-close type valve Vh4, back pressure regulator VPZ4 is connected with the entrance point of the 5th pillar, by the port of export of the 5th chromatographic column successively through open-close type valve Vh5, back pressure regulator VPZ5 is connected with the entrance point of first chromatographic column, the port of export of every chromatographic column is connected with one end of branch road stream transfer conduit (19) by Ve1, Ve2, Ve3, Ve4, Ve5 open-close type valve, the port of export of every chromatographic column is connected with extract pipeline (21) by Vf1, Vf2, Vf3, Vf4, Vf5 open-close type valve respectively, and the outlet of every pillar is connected with raffinate pipeline (20) by Vg1, Vg2, Vg3, Vg4, Vg5 open-close type valve respectively, the entrance point of every chromatographic column Z1, Z2, Z3, Z4, Z5 is connected with the other end of branch road stream transfer conduit (19) by open-close type valve Va1, Va2, Va3, Va4, Va5 separately respectively, and branch road stream transfer conduit (19) is provided with branch road transmission pump (22), back pressure regulator VPZ6, open-close type valve Vb1, Vb2, Vb3, Vb4, Vb5 are connected with injection port pipeline (16), open-close type valve Vc1, Vc2, Vc3, Vc4, Vc5 are connected with mobile phase entrance pipe (17), and open-close type valve Vd1, Vd2, Vd3, Vd4, Vd5 are connected with mobile phase entrance pipe (18), be connected to raffinate pipeline (20) upper, be connected to successively mass flowmenter F4, flow control valve VR4, back pressure regulating valve VPZ7, heated constant temperature groove (26), upper at extract pipeline (21), be connected to successively mass flowmenter F5, flow control valve VR5, back pressure regulating valve VPZ8, heated constant temperature groove (26), two heated constant temperature grooves (26) are connected with cyclone separator S1, S2 entrance respectively, the outlet at bottom of cyclone separator S1, S2 connects recycling can (30) by open-close type valve Vi1, Vi2 separately respectively, and the top outlet of cyclone separator S1, S2 connects back pressure regulating valve VPZ9, active carbon filter (27), cooler (29), mobile phase wet tank (1) after merging by check valve or open-close type valve respectively, after being connected to successively constant pressure pump (2), surge tank (3), heating thermostat (4) on the export pipeline of mobile phase wet tank (1), be connected with mobile phase carbon dioxide pipeline (9), mobile phase carbon dioxide pipeline (9) is connected with mobile phase carbon dioxide constant flow pump (11), (12), (14) arrival end by open-close type valve VK6, VK7, VK8 respectively, the modifier being provided by modifier tank (5) is connected with modifier constant flow pump (13), (15) arrival end respectively through modifier pipeline (8) by open-close type valve VK4, the port of export of mobile phase carbon dioxide constant flow pump (14), the port of export of modifier constant flow pump (15) are through pipeline be linked in sequence mixing chamber M1, flow control valve VR1, mass flowmenter F1 and mobile phase entrance pipe (18), the port of export of mobile phase carbon dioxide constant flow pump (12), the port of export of modifier constant flow pump (13) are through pipeline be linked in sequence mixing chamber M2, flow control valve VR2, mass flowmenter F2 and mobile phase entrance pipe (17), the feed liquid providing from material liquid tank (6) is connected with feed liquid constant flow pump (10) entrance with feed liquid pipeline (7) by open-close type valve VK5, and the port of export of mobile phase carbon dioxide constant flow pump (11), the port of export of feed liquid constant flow pump (10) are through pipeline be linked in sequence mixing chamber M3, flow control valve VR3, mass flowmenter F3 and injection port pipeline (16), mobile phase entrance pipe (18) is connected with chromatographic column Z1, Z2, Z3, Z4, Z5 arrival end through open-close type valve Vd1, Vd2, Vd3, Vd4, Vd5 respectively, mobile phase entrance pipe (17) is connected with chromatographic column Z1, Z2, Z3, Z4, Z5 arrival end through open-close type valve Vc1, Vc2, Vc3, Vc4, Vc5 respectively, injection port pipeline (16) is connected with chromatographic column Z1, Z2, Z3, Z4, Z5 arrival end through open-close type valve Vb1, Vb2, Vb3, Vb4 Vb5 respectively.
3. five districts series connection simulated movable bed chromatography devices according to claim 1, is characterized in that: described five districts' series connection simulated movable bed chromatography devices are located in system insulating box.
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| CN105572266A (en) * | 2016-03-04 | 2016-05-11 | 聊城大学 | Preparation supercritical fluid chromatographic instrument with multi-way valve and separation and purification method of preparation supercritical fluid chromatographic instrument |
| CN105784859A (en) * | 2016-03-04 | 2016-07-20 | 聊城大学 | Separation and purification preparation chromatograph and method for preparation, separation and purification |
| TWI610712B (en) * | 2016-05-19 | 2018-01-11 | 喬璞科技有限公司 | Series connected simulated moving bed 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 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105572266A (en) * | 2016-03-04 | 2016-05-11 | 聊城大学 | Preparation supercritical fluid chromatographic instrument with multi-way valve and separation and purification method of preparation supercritical fluid chromatographic instrument |
| CN105784859A (en) * | 2016-03-04 | 2016-07-20 | 聊城大学 | Separation and purification preparation chromatograph and method for preparation, separation and purification |
| TWI610712B (en) * | 2016-05-19 | 2018-01-11 | 喬璞科技有限公司 | Series connected simulated moving bed 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 |
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| WO2020258705A1 (en) * | 2019-06-28 | 2020-12-30 | 信达生物制药(苏州)有限公司 | Modular chromatography device |
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