CN101822914B - High-efficiency liquid-phase preparation device of axial pressurizing chromatographic column - Google Patents
High-efficiency liquid-phase preparation device of axial pressurizing chromatographic column Download PDFInfo
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- CN101822914B CN101822914B CN2010101538545A CN201010153854A CN101822914B CN 101822914 B CN101822914 B CN 101822914B CN 2010101538545 A CN2010101538545 A CN 2010101538545A CN 201010153854 A CN201010153854 A CN 201010153854A CN 101822914 B CN101822914 B CN 101822914B
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Abstract
The invention provides an axial pressurizing chromatographic column device for a high performance liquid preparation chromatography, relates to the technical field of chromatography liquid-phase preparation. The invention comprises a main frame, an axial pressurizing chromatographic column body, a loading oil cylinder and a pressurizing hydraulic station. The invention is characterized by also comprising a chromatographic column oscillating mechanism. The axial pressurizing chromatographic column body is connected to the main frame through the chromatographic column oscillating mechanism. A hydraulic energy accumulator is also arranged on a hydraulic loop between the loading oil cylinder and the pressurizing hydraulic station. The axial pressurizing chromatographic column body comprises a chromatographic column shell, an upper end cover and a piston body assembly, and the lower end of the chromatographic column is connected with the loading oil cylinder through a flange assembly. The invention greatly improves the yield and the purity of a product, prolongs the service life of the chromatographic column, and can automatically and repeatedly fill, thereby saving the production cost.
Description
Technical field
The present invention relates to chromatography preparation technique of liquid phase field, specifically a kind of device of axial pressurizing chromatographic column that is used for high performance liquid preparative chromatography.
Background technology
High performance liquid chromatography, be a kind of utilize material two mutually in absorption or the fine difference of distribution coefficient reach the method that the purpose of separation is separated.When material when two relatively move mutually, measured matter carries out repeated dispensing mutually two, makes original small distribution difference produce the effect of amplifying like this, thereby reaches separation, analyzes and measure the purpose of some physicochemical constants.
Chromatographic column is the core apparatus that high performance liquid chromatography is produced process, and the leading indicator of wherein weighing the post effect is a height equivalent to a theoretical plate, and for given filler, post is imitated fill method and the column length that mainly depends on pillar.If the selection appropriate method just can obtain higher post and imitate with short chromatographic column, both can practice thrift cost of equipment, also can save operation expense (, improving recovery rate etc.) such as the consumption that can reduce solvent.
When liquid phantom preparing chromatogram is used, should make its post imitate as far as possible near or the post that reaches when analyzing chromatographic column and loading solid phase filler of the same race imitate.Generally, post is imitated with granularity and the size of solid phase filler proportional, can according to the post that will reach imitate the size of selecting filler, also can adjust the post effect through the size of filler.Select cheap coarse filler, can reduce the operating pressure of pillar, use more cheap low-lift pump can satisfy the operation requirement, also lower but its post is imitated.On the contrary, the uniform solid phase filler if select less can obtain higher post and imitate, but this will improve the operating pressure of pillar usually.Therefore, when the solid phase filler granularity of using is certain, how improves post as much as possible and imitate, can become the problem of selecting post to press eclectically to a certain extent.A kind of chromatographic column device that is used for liquid phase production that my company has developed; Not only good solution is provided in this aspect; The simultaneously integrated advanced technology of mechanical electronic hydraulic instantly a lot, the post that improves the preparative chromatography post is imitated a lot of solutions is provided, and among trying out.
Summary of the invention
The object of the present invention is to provide a kind of device of axial pressurizing chromatographic column that is used for high performance liquid preparative chromatography,, increase the service life, and can load repeatedly, save production cost to improve product yield and purity.
The present invention solves the technical scheme that its technical problem takes: a kind of device of axial pressurizing chromatographic column that is used for high performance liquid preparative chromatography; Comprise main frame, axial pressurizing chromatographic column body, load cylinder and pressurized hydraulic station; It is characterized in that; Also comprise the chromatographic column oscillating mechanism that in the three dimensions of vertical direction and side direction, to swing; Said axial pressurizing chromatographic column body is connected on the main frame through the chromatographic column oscillating mechanism, and said axial pressurizing chromatographic column body lower end is connected with load cylinder through flange assembly; On the hydraulic circuit between said load cylinder and the pressurized hydraulic station, also be provided with hydraulic accumulator;
Said axial pressurizing chromatographic column body is made up of chromatographic column housing, upper end cover, piston body assembly;
Said chromatographic column oscillating mechanism comprises mounting platform, spring oscillation device and hinge oscillation device; Said mounting platform is fixed on the main frame; Mounting spring oscillation device on the said mounting platform, described spring oscillation device comprise upper flat plate, following flat board, column and back-moving spring; Be positioned at the upper flat plate at column two ends, following dull and stereotyped upside and the downside that is distributed in mounting platform respectively, said back-moving spring is between upper flat plate and mounting platform; Said hinge oscillation device is installed on the following flat board of spring oscillation device; Said hinge oscillation device comprises bearing block, hinge; Said bearing block is installed on the following flat board of spring oscillation device, and hinge is rotatable to be arranged in the bearing block, and simultaneously said hinge connects axial pressurizing chromatographic column body; Above-mentionedly know that the integral installation of hinge oscillation device is on the following flat board of spring oscillation device, with a dull and stereotyped oscillates down.
Said piston body assembly comprises piston body; And said piston body axially has the through hole that is communicated with inside and outside two side ends; The inboard end face of said piston body is arranged inlet convergence plate, inlet screen and the first pilot seal cover successively, and said first pilot seal cover is fixed on the inboard end of piston body with inlet convergence plate, inlet screen; The said piston body outside is nested with the second pilot seal cover; Be provided with general plug envelope sealing ring on the said piston body and between first pilot seal cover; Be provided with seal with O ring on the said piston body and between second pilot seal cover.
In order to limit the rotation amplitude of hinge, can between said bearing block and hinge, set up a limiting plate assembly.
Described hydraulic energy storage device is that bag type accumulator is used in pressurize.
The surface roughness Ra of said chromatographic column inner walls≤0.25 μ m.
The invention has the beneficial effects as follows:
1) post is imitated height, and favorable reproducibility is loaded used time weak point.Can adopt the littler filler of particle diameter, reduce column length, increase the post footpath, thereby reduce waller effect, can obtain almost imitating, thereby can make purification efficiency higher near the post of analytical column.The filling process is easy to learn, even without contacted people, also can learn very soon.After chromatographic column is in a single day contaminated, can be easily, discharging easily, filling again again.
2) in axial pressure preparative chromatography column method, my company has adopted the pressurize measure of accumulator in the control of hydraulic coupling, makes in the cylinder piston body type as the compression spring, imposes on the bed constant compression force.Column cap all closely contacts with bed with piston end, and the chromatographic column two ends can not take place loosening and form the hole.In chromatographic column works long hours process, still have constant compression force to act on piston, post is imitated can keep stable for a long time.And not between the operating period, space that forms in the post or crack still can obtain initial post and imitate after pressurization recovers.
3) axial pressure preparative chromatography column technology has solved the scale-up problem of preparative chromatography technology basically.For the preparative column of 10 μ m fillers, its effective plate number is more than the 40000/m, and the symmetry value at peak is 0.9～1.2; Behind the reduced plate height (ratio of actual plate hight and filler particles diameter); The post effect almost post effect with analytical column is the same high, can directly amplify, and saves time and cost.
In sum, axial pressure preparative chromatography post has improved the yield and the purity of product greatly, has prolonged the service life of chromatographic column, and can oneself load repeatedly, saves production cost.
Description of drawings
Fig. 1 is the structure chart of the present invention behind the omission main frame;
Fig. 2 is that the A of Fig. 1 is to diagrammatic sketch;
Fig. 3 oscillating mechanism part-structure figure;
Fig. 4 is a piston body assembly profile;
Among the figure: 1 main frame, 2 axial pressurizing chromatographic column body, 21 chromatographic column housings, 22 upper end covers, 24 flange assemblies, 25 sphere joint connectors; 3 load cylinders, 41 mounting platforms, 42 upper flat plates, 43 times flat boards, 44 columns, 45 back-moving springs; 46 bearing blocks, 47 hinges, 51 piston bodies, 52 through holes, 53 inlet convergence plate; 54 inlet screens, 55 first pilot seal covers, 56 second pilot seal covers, 57 general plug envelope sealing rings, 58 seal with O rings.
The specific embodiment
Like Fig. 1～shown in Figure 4, a kind of device of axial pressurizing chromatographic column that is used for high performance liquid preparative chromatography comprises main frame 1, axial pressurizing chromatographic column body 2, load cylinder 3 and pressurized hydraulic station, also comprises chromatographic column oscillating mechanism, hydraulic accumulator; Said axial pressurizing chromatographic column body 2 is connected on the main frame 1 through oscillating mechanism; Said hydraulic energy storage device is installed on the hydraulic circuit between load cylinder and the pressurized hydraulic station, constitutes hydraulic control circuit jointly.Owing to connect through hydraulic circuit between load cylinder and the pressurized hydraulic station, so the pressurized hydraulic station can be installed in any suitable position.
Main frame 1 structure all adopts the rectangular tube stainless steel to be welded, and people from station platform and last helper are set as required in the above.
Said axial pressurizing chromatographic column body 2 is made up of chromatographic column housing 21, upper end cover 22, flange assembly 24, piston body assembly, and said axial pressurizing chromatographic column body 2 lower ends are connected with load cylinder 3 through flange assembly 24.Said piston body assembly comprises piston body 51; And said piston body axially has the through hole 52 that is communicated with inside and outside two side ends; Said piston body 51 inboard end faces are arranged inlet convergence plate 53, inlet screen 54 and first pilot seal cover 55 successively, and said first pilot seal cover is fixed on the inboard end of piston body with inlet convergence plate, inlet screen; Said piston body 1 outside is nested with second pilot seal cover 56; Be provided with general plug envelope sealing ring 57 on the said piston body and between first pilot seal cover; Be provided with seal with O ring 58 on the said piston body 51 and between second pilot seal cover 56.These parts promptly are the parts of the application of force, are also carrying the effect of appearance inlet and movable sealing.First road adopts general plug envelope sealing ring, and the big seal with O ring of decrement is adopted in the sealing of second road, forms redundant double sealing, guarantees the zero leakage of piston.Simultaneously; Also be serially connected with sphere joint connector 25 between axial pressurizing chromatographic column body 2 and the load cylinder 3; This sphere joint connector 25 comprises spherical connecting body and adapter sleeve; Said spherical connecting body cooperates through sphere with adapter sleeve realizes that three-dimensional activity is connected, and has certain three-dimensional activity space, is used for the small compensation of the concentricity alignment error of compensating axial pressurizing chromatographic column body and load cylinder.Replace being rigidly connected and help strengthening the movable sealing effect of axial pressurizing chromatographic column body and oil cylinder.
The surface roughness Ra of said chromatographic column inner walls≤0.25 μ m.
Said chromatographic column oscillating mechanism comprises mounting platform 41, spring oscillation device and hinge oscillation device; Said mounting platform 41 is fixed on the main frame 1; Mounting spring oscillation device on the said mounting platform 41; Described spring oscillation device comprises upper flat plate 42, following flat board 43, column 44 and back-moving spring 45; Be positioned at the upper flat plate at column two ends, following dull and stereotyped upside and the downside that is distributed in mounting platform 41 respectively, back-moving spring 45 is between upper flat plate and mounting platform; Said hinge oscillation device is installed on the following flat board of spring oscillation device.Said hinge oscillation device comprises bearing block 46, hinge 47; Said bearing block 46 be installed in the spring oscillation device following dull and stereotyped 43 on, hinge is rotatable to be arranged in the bearing block, simultaneously hinge connects axial pressurizing chromatographic column body; Above-mentionedly know that the integral installation of hinge oscillation device is on the following flat board of spring oscillation device, with a dull and stereotyped oscillates down.In order to limit the rotation amplitude of hinge, can between said bearing block and hinge, set up a limiting plate assembly.
Described hydraulic energy storage device preferentially adopts pressurize to use bag type accumulator.
Except that the described technical characterictic of specification, be the known technology of those skilled in the art.
Claims (4)
1. device of axial pressurizing chromatographic column that is used for high performance liquid preparative chromatography; Comprise main frame, axial pressurizing chromatographic column body, load cylinder and pressurized hydraulic station; It is characterized in that; Also comprising can be at the chromatographic column oscillating mechanism of vertical direction and the swing of side direction three dimensions, and said axial pressurizing chromatographic column body is connected on the main frame through the chromatographic column oscillating mechanism, and said axial pressurizing chromatographic column body lower end is connected with load cylinder through flange assembly; On the hydraulic circuit between said load cylinder and the pressurized hydraulic station, also be provided with hydraulic accumulator;
Said axial pressurizing chromatographic column body is made up of chromatographic column housing, upper end cover, piston body assembly;
Said chromatographic column oscillating mechanism comprises mounting platform, spring oscillation device and hinge oscillation device; Said mounting platform is fixed on the main frame; Mounting spring oscillation device on the said mounting platform; Described spring oscillation device comprises upper flat plate, following flat board, column and back-moving spring; Be positioned at the upper flat plate at column two ends, upside and the downside that time flat board is distributed in mounting platform, said back-moving spring is between upper flat plate and mounting platform; Said hinge oscillation device is installed on the following flat board of spring oscillation device; Said hinge oscillation device comprises bearing block, hinge; Said bearing block is installed on the following flat board of spring oscillation device, and said hinge is rotatable to be arranged in the bearing block, and simultaneously said hinge connects axial pressurizing chromatographic column body.
2. a kind of device of axial pressurizing chromatographic column that is used for high performance liquid preparative chromatography according to claim 1; It is characterized in that; Said piston body assembly comprises piston body; And said piston body axially has the through hole that is communicated with inside and outside two side ends, and the inboard end face of said piston body is arranged inlet convergence plate, inlet screen and the first pilot seal cover successively, and said first pilot seal cover is fixed on the inboard end of piston body with inlet convergence plate, inlet screen; The said piston body outside is nested with the second pilot seal cover; Be provided with general plug envelope sealing ring on the said piston body and between first pilot seal cover; Be provided with seal with O ring on the said piston body and between second pilot seal cover.
3. a kind of device of axial pressurizing chromatographic column that is used for high performance liquid preparative chromatography according to claim 1 is characterized in that, described hydraulic energy storage device is that bag type accumulator is used in pressurize.
4. a kind of device of axial pressurizing chromatographic column that is used for high performance liquid preparative chromatography according to claim 1 is characterized in that, the surface roughness Ra of said chromatographic column inner walls≤0.25 μ m.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2010101538545A CN101822914B (en) | 2010-04-23 | 2010-04-23 | High-efficiency liquid-phase preparation device of axial pressurizing chromatographic column |
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| CN2010101538545A CN101822914B (en) | 2010-04-23 | 2010-04-23 | High-efficiency liquid-phase preparation device of axial pressurizing chromatographic column |
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| CN101822914A CN101822914A (en) | 2010-09-08 |
| CN101822914B true CN101822914B (en) | 2012-03-21 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102989199B (en) * | 2012-12-11 | 2014-09-03 | 聊城万合工业制造有限公司 | Inner storage constant-pressure preparative column device |
| CN113915177B (en) * | 2021-09-16 | 2024-05-14 | 利穗科技(苏州)有限公司 | Electrohydraulic servo driving device and chromatographic equipment |
| CN116585752B (en) * | 2023-07-18 | 2023-10-20 | 成都百泉生物医药科技有限公司 | Chromatographic column and oscillating device for chromatographic column |
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| DE19903255C1 (en) * | 1999-01-28 | 2000-04-13 | Infraserv Gmbh & Co Hoechst Kg | Chromatography column comprises lid, seat and base, and can be rotated about axis |
| CN201022992Y (en) * | 2007-04-13 | 2008-02-20 | 成都普思生物科技有限公司 | Axial pressure high performance liquid chromatographic column |
| CN201692692U (en) * | 2010-04-23 | 2011-01-05 | 聊城万合工业制造有限公司 | High-performance liquid preparation device for axial pressurization chromatographic column |
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