CN104399271B - The online enrichment facility of component and control procedure after chromatographic column post - Google Patents
The online enrichment facility of component and control procedure after chromatographic column post Download PDFInfo
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- CN104399271B CN104399271B CN201410778311.0A CN201410778311A CN104399271B CN 104399271 B CN104399271 B CN 104399271B CN 201410778311 A CN201410778311 A CN 201410778311A CN 104399271 B CN104399271 B CN 104399271B
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Abstract
The online enrichment facility of component and control procedure after chromatographic column post, its concentration tank inner chamber is divided into multiple concentrated chamber side by side; Drainer is fixedly located at concentration tank tail end; Detector flow cell entrance connects chromatographic column; The outlet of detector flow cell is connected to upper end, concentration tank each concentrated chamber, to the branch road in each concentrated chamber, establish magnetic valve; Discharge gate is established respectively in the lower end in each concentrated chamber; Thermal medium pump is communicated to lower end, each concentrated chamber; Negative pressure pump is communicated to each concentrated chamber and drainer cavity upper end; Cold medium pump is communicated to drainer inner chamber lower end; Drainer row mouth is communicated with regenerated solvent tank.It can realize online recycling that is online concentrated and chemical solvent to liquid after chromatographic column, not only improve thickening efficiency, and not by the restriction of liquid stock size after chromatographic column post time concentrated, whole process is carried out in sealed environment, is applicable to the extraction of the object concentrate of easy oxidation deterioration.And the impurity produced is recycled, avoid the pollution to environment.
Description
Technical field
The present invention relates to the correlative technology field of pharmaceutical equipment, particularly in natural Chinese medicinal herb, designative species, liquid component separation, concentrated, removal process application apparatus, the specifically online enrichment facility of component after a kind of chromatographic column post.
Background technology
Based on the chromatographic purification methods of liquid chromatography technology, be applied to chemical industry, medical industry in recent years, realize getting purer object from a large amount of admixture solvent.Because the method has advanced tester and the intervention of electronic computer, make this method very reliable, be more and more subject to the welcome of professional person.
At present, apply chromatographic column in production and carry out in the process of purifies and separates, a large amount of chemical solvents can be used as mobile phase.Liquid after being called as post from the mobile phase of chromatographic column tail end outflow.Different liquid components is had in liquid after post in the different time.Wherein, after the post containing different target thing liquid and containing impurity post after liquid all to shunt, collect respectively.After shunting, different objects and impurity are all miscible among the chemical solvent of mobile phase using very little concentration (generally can be less than 5g/L).
At present, the enterprise that output is very large concentrates after generally liquid after the post of same component being stored into certain amount and concentrates in distillation still.The enterprise that output is very little then uses Rotary Evaporators to concentrate.Both features are respectively: distillation still single treatment amount is large, and lossy, easily occur cross pollution, equipment cost is higher.Rotary Evaporators single treatment amount is too small, expends time in, and often goes out of use containing liquid after the post of impurity, contaminated environment.Meanwhile, two kinds of processing modes are all not suitable for the object of easy oxidation deterioration.
Summary of the invention
The invention provides the online enrichment facility of component after a kind of chromatographic column post, it is by means of liquid chromatography technology, realize carrying out concentration extraction to liquid after chromatographic column post online, the size of the real-time generation of liquid after chromatographic column post need not be distinguished, and differentiation recovery can be carried out to impurity.
The present invention solves the technical scheme that its technical problem takes:
The online enrichment facility of component after a kind of chromatographic column post, comprises detector flow cell, concentration tank, drainer, thermal medium pump, negative pressure pump, cold medium pump, regenerated solvent tank and control unit; The lumen segmentation of described concentration tank is multiple concentrated chamber side by side; Described drainer is fixedly installed on the tail end of described concentration tank; The entrance of described detector flow cell is communicated with the port of export of chromatographic column; The outlet of described detector flow cell is communicated to the upper end, each concentrated chamber of concentration tank respectively, and is arranging magnetic valve respectively to the branch road in each concentrated chamber; Described each magnetic valve, thermal medium pump, negative pressure pump, cold medium pump and detector flow cell all connect described control unit; In the lower end in each concentrated chamber of described concentration tank, discharge gate is set respectively; Described thermal medium pump is communicated to the lower end in each concentrated chamber of described concentration tank; Described negative pressure pump is communicated to the upper end in each concentrated chamber of described concentration tank and the upper end of described drainer cavity; Described cold medium pump is communicated to the inner chamber lower end of described drainer; The lower end Pai Kou of described drainer is communicated to described regenerated solvent tank.
Described concentration tank is that impurity concentrates chamber in the concentrated chamber of throughput direction (namely direction) from right to left end.
What described control unit adopted is Programmable Logic Controller.Between described concentration tank and the contact wall of described drainer, thermal insulation layer is set, reduce the condensation of drainer and impurity concentrate thermal evaporation in chamber between the degree that influences each other, guarantee the physical action effect of condensation in two chambeies, heating and gasifying separately, reduce energy consumption.
After described chromatographic column post, the control procedure of the online enrichment facility of component is:
Thermal medium pump constantly carries out heat supply to each concentrated chamber of concentration tank; Negative pressure pump constantly runs and vacuumizes each concentrated chamber of concentration tank simultaneously; Cold medium pump is constantly freezed to drainer;
Detect at detector flow cell after entering detector flow cell containing the liquid flux of different component by chromatographic column, detecting as being opened by the magnetic valve at concentrated chamber place corresponding in control unit control concentration tank during a certain concentration components, making other closed electromagnetic valves simultaneously; But when concentration components not detected, the magnetic valve controlling to be in concentration tank the concentrated chamber place of throughput direction end by control unit is opened, and makes other closed electromagnetic valves simultaneously.
The invention has the beneficial effects as follows: it can realize online recycling that is online concentrated and chemical solvent to liquid after chromatographic column, not only improve thickening efficiency, and not by the restriction of liquid stock size after chromatographic column post time concentrated, whole process is carried out in sealed environment, is applicable to the extraction of the object concentrate of easy oxidation deterioration.And the impurity produced is recycled, avoid the pollution to environment.
Accompanying drawing explanation
Fig. 1 is structural representation of the present invention;
In figure: 1 chromatographic column, 2 detector flow cells, 3A concentrates chamber, and 4B concentrates chamber, and 5C concentrates chamber, and 6D concentrates chamber, and 7 impurity concentrate chamber, 8 drainers, 9 thermal medium pumps, 10 negative pressure pumps, 11 cold medium pump, 12 regenerated solvent tanks.
Detailed description of the invention
For ease of understanding technical scheme of the present invention, below in conjunction with accompanying drawing, wherein involved technology contents is described further.
In the description of this invention, it should be noted that, term "left", "right", " on ", D score, " interior ", the orientation of the instruction such as " outward " or position relationship be based on orientation shown in the drawings or position relationship, only the present invention for convenience of description and simplified characterization, instead of indicate or imply that the device of indication or element must have specific orientation, with specific azimuth configuration and operation, therefore can not be interpreted as limitation of the present invention.
In describing the invention, it should be noted that, unless otherwise clearly defined and limited, term " installation ", " being connected ", " connection " should be interpreted broadly, and such as, can be fixedly connected with, also can be removably connect, or connect integratedly; Can be mechanical connection, also can be electrical connection, can be directly to be connected, and also indirectly can be connected by intermediary, can be the connection of two element internals.For the ordinary skill in the art, concrete condition above-mentioned term concrete meaning in the present invention can be understood.
As shown in Figure 1:
The online enrichment facility of component after a kind of chromatographic column post, it comprises detector flow cell 2, concentration tank, drainer 8, thermal medium pump 9, negative pressure pump 10, cold medium pump 11, regenerated solvent tank 12 and control unit.
The inner chamber of described concentration tank is divided into five concentrated chambeies side by side in the lateral direction, is that A concentrates chamber 3, B concentrates chamber 4, C concentrates chamber 5, D concentrates chamber 6 and impurity concentrates chamber 7.Described drainer 8 is fixedly installed on the tail end (i.e. left end, because negative pressure pump 10 pumping direction arranged is from right to left, so the left end of concentration tank is called tail end) of described concentration tank.The entrance of described detector flow cell 2 is communicated with the port of export of chromatographic column 1.The outlet of described detector flow cell 2 is communicated to the upper end, each concentrated chamber of concentration tank respectively, and to the branch road in each concentrated chamber, magnetic valve is set respectively, corresponding described A concentrates chamber 3, B concentrates chamber 4, C concentrates chamber 5, D concentrates chamber 6 and impurity concentrate chamber 7 respectively called after valve, No. two valves, No. three valves, No. four valves, No. five valves.Described each magnetic valve, thermal medium pump 9, negative pressure pump 10, cold medium pump 11 and detector flow cell 2 all connect described control unit.Arrange discharge gate respectively in the lower end in each concentrated chamber of described concentration tank, concentrated A concentrate, B concentrate, C concentrate, D concentrate and the impurity obtained inputs corresponding receiving flask by each discharge gate.
Described thermal medium pump 9 is arranged on the right-hand member of described concentration tank, and is communicated to the lower end in each concentrated chamber of described concentration tank, and pumping into direction is right-to-left.Described negative pressure pump 10 is arranged on the left end of described concentration tank, and is communicated to the upper end of described concentration tank each concentrated chamber cavity, described drainer 11 cavity, and sucking-off direction is right-to-left.Described cold medium pump 11 is communicated to the inner chamber lower end of described drainer 8.The lower end Pai Kou of described drainer 8 is communicated to described regenerated solvent tank 12.
Described control unit can adopt Programmable Logic Controller.Benefit arranges thermal insulation layer between described concentration tank and the contact wall of described drainer 8.
General principle: each concentrated chamber that described thermal medium pump is concentration tank provides circulation thermal source, makes to enter the mobile phase solvent gasification 90% in liquid after the post in each concentrated chamber.Negative pressure pump 10 makes the solvent gas in each concentrated chamber after gasification enter in drainer 8 cavity, meanwhile, makes each concentrated chamber produce negative pressure to reduce the gasification temperature of solvent.Cold medium pump 11 to circulate cooling for drainer 8, the solvent of gasification is liquefied again, and flows into regenerated solvent tank, use as mobile phase.Each component, after each concentrated chamber realization of described concentration tank is concentrated, flows out from concentrated solution outlet, enters corresponding concentrate receiving flask.
General work method: during with solvent after the post of different component by described detector flow cell, the concentrated chamber that solvent after tested flows into regulation according to technological order concentrates, and makes the concentrate obtained enter corresponding receiving flask, is specially:
When described detector flow cell 2 does not detect and needs component, No. five valves are in normally open, other solenoid closures, and waste liquid enters impurity and concentrates in chamber 7 and be separated into regenerated solvent and impurity.
When there is component A (A concentrate) after described detector flow cell 2 detects post in solvent, a valve is opened, other solenoid closures, and component A enters A and concentrates in chamber 3 and be separated into regenerated solvent and A concentrate.Regenerated solvent is evacuated in drainer chamber 8 by negative pressure pump 10, and A concentrate enters receiving flask.
When there is B component in solvent after described detector flow cell 2 detects post, No. two valves are opened, other solenoid closures, and B component enters B and concentrates in chamber 4 and be separated into regenerated solvent and B concentrate.In like manner, regenerated solvent is evacuated in drainer chamber by negative pressure pump 10, and B concentrate enters receiving flask.
Be suitable for by that analogy component C, D component concentrated etc.
After conventional chromatographic column post, the concentration tank of the online enrichment facility of component is generally 5 to 8 concentrated chambeies, and according to liquid property, each concentrated chamber arranges in turn according to the order of flow direction, and impurity concentrates chamber to arrange in end with drainer 8 by neighbour.
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the prerequisite not departing from the technology of the present invention principle; can also make some improvement and modification, these improve and modification also should be considered as protection scope of the present invention.
Except the technical characteristic described in description, be the known technology of those skilled in the art.
Claims (5)
1. the online enrichment facility of component after chromatographic column post, is characterized in that:
Comprise detector flow cell, concentration tank, drainer, thermal medium pump, negative pressure pump, cold medium pump, regenerated solvent tank and control unit;
The lumen segmentation of described concentration tank is multiple concentrated chamber side by side;
Described drainer is fixedly installed on the tail end of described concentration tank;
The entrance of described detector flow cell is communicated with the port of export of chromatographic column;
The outlet of described detector flow cell is communicated to the upper end, each concentrated chamber of concentration tank respectively, and is arranging magnetic valve respectively to the branch road in each concentrated chamber;
Described each magnetic valve, thermal medium pump, negative pressure pump, cold medium pump and detector flow cell all connect described control unit;
In the lower end in each concentrated chamber of described concentration tank, discharge gate is set respectively;
Described thermal medium pump is communicated to the lower end in each concentrated chamber of described concentration tank;
Described negative pressure pump is communicated to the upper end in each concentrated chamber of described concentration tank and the upper end of described drainer cavity;
Described cold medium pump is communicated to the inner chamber lower end of described drainer;
The lower end Pai Kou of described drainer is communicated to described regenerated solvent tank.
2. the online enrichment facility of component after chromatographic column post according to claim 1, is characterized in that: described concentration tank is that impurity concentrates chamber in the concentrated chamber of throughput direction end.
3. the online enrichment facility of component after chromatographic column post according to claim 1 and 2, is characterized in that: what described control unit adopted is Programmable Logic Controller.
4. the online enrichment facility of component after chromatographic column post according to claim 1 and 2, is characterized in that: between described concentration tank and the contact wall of described drainer, arrange thermal insulation layer.
5. based on the control procedure of the online enrichment facility of component after chromatographic column post described in claim 1,
Thermal medium pump constantly carries out heat supply to each concentrated chamber of concentration tank; Negative pressure pump constantly runs and vacuumizes each concentrated chamber of concentration tank simultaneously; Cold medium pump is constantly freezed to drainer;
Detect at detector flow cell after entering detector flow cell containing the liquid flux of different component by chromatographic column, detecting as being opened by the magnetic valve at concentrated chamber place corresponding in control unit control concentration tank during a certain concentration components, making other closed electromagnetic valves simultaneously; But when concentration components not detected, the magnetic valve controlling to be in concentration tank the concentrated chamber place of throughput direction end by control unit is opened, and makes other closed electromagnetic valves simultaneously.
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| CN201410778311.0A CN104399271B (en) | 2014-12-15 | 2014-12-15 | The online enrichment facility of component and control procedure after chromatographic column post |
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| CN201410778311.0A CN104399271B (en) | 2014-12-15 | 2014-12-15 | The online enrichment facility of component and control procedure after chromatographic column post |
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| CN104399271A CN104399271A (en) | 2015-03-11 |
| CN104399271B true CN104399271B (en) | 2016-01-20 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US6149136A (en) * | 1998-01-20 | 2000-11-21 | Air Products And Chemicals, Inc. | Distributor for packed liquid-vapor contact column |
| JP5186807B2 (en) * | 2007-05-28 | 2013-04-24 | 株式会社日立プラントテクノロジー | Liquid concentration system |
| CN201200820Y (en) * | 2008-04-10 | 2009-03-04 | 河源新丽宝轻烃能源科技发展有限公司 | Gas-mixing pot for evaporation of light hydrocarbon |
| CN203469510U (en) * | 2013-10-04 | 2014-03-12 | 昆明赛诺制药有限公司 | Spherical vacuum concentrating pan |
| CN204428861U (en) * | 2014-12-15 | 2015-07-01 | 聊城万合工业制造有限公司 | The online enrichment facility of component after chromatographic column post |
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