CN101091840A - Refluent chromatogram method and equipment with excentric multiple channels - Google Patents

Refluent chromatogram method and equipment with excentric multiple channels Download PDF

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Publication number
CN101091840A
CN101091840A CN 200710068115 CN200710068115A CN101091840A CN 101091840 A CN101091840 A CN 101091840A CN 200710068115 CN200710068115 CN 200710068115 CN 200710068115 A CN200710068115 A CN 200710068115A CN 101091840 A CN101091840 A CN 101091840A
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China
Prior art keywords
splitter
hollow shaft
adverse current
tube
current chromatogram
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CN 200710068115
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Chinese (zh)
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CN101091840B (en
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吴世华
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Zhejiang University ZJU
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Zhejiang University ZJU
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Publication of CN101091840B publication Critical patent/CN101091840B/en
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Abstract

The invention publishes an equipment and method for eccentric multichannel adverse current chromatograph. It uses three or more than three lead-in tubes and extraction tubes which is respectively independent of separation column with hollow axle partially distributed according to the same connection mode parallel connection, complete the independent chromatograph operation of each separation column. The equipment includes the separation column which may revolute by passing the fixing hollow axle center of the box body center and simultaneously synchronism rotate by passing the separation column canon center, of which the hollow axle of separation column with symmetric distribution at least has two, there is at least two separation columns with the separation column hollow axle bias distributed on each hollow axle of the separation column, all separation columns through respectively independent lead-in tube and extraction tubes parallel connected. The invention may effectively raise space utilance and analysis preparation ability of single plane, especially qualify industrialization parallel separation.

Description

The multichannel adverse current chromatogram method and apparatus of a kind of off-centre
Technical field
The present invention relates to counter-current chromatograph, relate to the counter-current chromatograph that a kind of liquid-liquid two phase countercurrent flow that does not have solid-state carrier distributes specifically.
Background technology
Adverse current chromatogram is a kind of liquid liquid partition chromatography without solid-state carrier.Owing to its no Irreversible Adsorption, rate of recovery height, sample are difficult for characteristics such as destroyed, that solvent consumption is few, and be subjected to organic chemist, inorganic chemist, Pharmaceutical Chemist, biochemists' great attention day by day.Adverse current chromatogram has been classified as a kind of important separation and purification means in the world, and be widely used in the separation and purification of natural products and synthesis of chemicals.High-speed counter-current chromatograph commonly used, helix tube is coaxially on supporter, under the effect of its special centrifugal force field, forming unidirectional two-phase distributes, thereby realize the fixedly high retention of phase, can use the big flow wash-out of high flow velocities, allocative efficiency is also higher, thereby high-speed counter-current chromatograph not only develops into the common instrument of analytic type, and prepares aspect such as type at half preparation, preparation type and big capacity and all obtained great application.But up to the present, all kinds of high-speed counter-current chromatographs all only can provide one or both chromatographic isolation simultaneously, are difficult to satisfy the chromatographic isolation requirement of the parallel preparation in multipotency road.
United States Patent (USP) 5,024,758 disclose a kind of centering type horizontal flow general formula counter-current chromatograph, are provided with although splitter is eccentric, and its instrument can only provide a kind of chromatographic isolation.United States Patent (USP) 5,217,608 " the planetary centrifugal chromatographies of multicolumn ", Chinese patent ZL00207386.2 " many splitters high-speed counter-current chromatograph " and ZL02261047.2 " high-speed counter-current chromatograph " disclose the different many splitters counter-current chromatograph of several structures respectively.These counter-current chromatographs all adopt the same structure of a plurality of series connection and the splitter of same capability, although improved the balance quality of instrument greatly, have increased the preparative capacibility of unit, instrument can only provide a kind of adverse current chromatogram look from.For high flux, large-scale parallel preparation, have to adopt many to dispose parallel the carrying out of counter-current chromatograph that same motor, housing are conciliate the winch structure, greatly increased operating cost, increased the risk and the labour intensity of experiment simultaneously.Chinese patent ZL02223866.2 " a kind of twin columns counter-current chromatograph " and ZL03229896.X " the at a high speed contrary extra large chromatograph of multi-functional compatible type " disclose a kind of compatible high-speed counter-current chromatograph with two splitters, though be easy to change splitter and change the splitter parameter, but complicated pipelines compile bundle mode and limited instrument utilize spatial constraints its apply, also be difficult to satisfy simultaneously multichannel parallel preparation separation requirement.
Summary of the invention
The objective of the invention is to be to overcome the deficiency of present above-mentioned adverse current chromatogram method and apparatus, and a kind of new eccentric multichannel adverse current chromatogram method and apparatus is provided.
Technical problem of the present invention is solved by following technical proposals.
The multichannel adverse current chromatogram method of off-centre of the present invention, inlet tube is connected according to identical connected mode is parallel in the same way with fairlead with using separately independently with the splitter of splitter hollow shaft decentered distribution more than three or three in employing, makes each splitter finish independently chromatographic run.
The adverse current chromatogram equipment that is used for above-mentioned eccentric multichannel adverse current chromatogram method and designs, comprise casing, can be around the revolution of the fixation hollow axle center at casing center simultaneously again around the splitter hollow shaft central synchronous splitter of rotation in the same way, and the inlet tube that is connected with splitter, fairlead and for prevent that the inlet tube fairlead from beating strand with the paired synchronous reverse rotation of splitter hollow shaft separate the strand open tubular column, it is characterized in that having two or more splitter hollow shafts of symmetrical distribution, each splitter hollow shaft is provided with the splitter of two or more and splitter hollow shaft decentered distribution, all splitters by separately independently inlet tube be connected with fairlead is parallel in the same way.
Further feature of the present invention, said splitter are the spiral tubes that is formed according to hand of spiral coiling by separator tube, or the coiling tubing string that is formed according to the coil direction coiling by separator tube.
Said separator tube is polyfluortetraethylene pipe, stainless steel tube or glass tube.The cross section of separator tube can be circle, rectangle or square.The inwall of separator tube can or be screw-like or corrugated for the plane.
Among the present invention, the preparation capacity of said splitter is analytic type, half preparation type, preparation type or industrial production type.Usually, in casing, be provided with the heating module of control separation temperature.
Beneficial effect of the present invention is:
The splitter of parallel eccentric installing has reduced the emulsifying effectiveness of system, is particularly suitable for the parallel preparation of high flux of large biological molecule.This set, analysis, the preparative capacibility of unit have not only been improved, and improved the production efficiency of unit interval greatly, reduced operating cost, be particularly suitable for extensive, the high-throughout parallel analysis and the preparation of biological sample, be particularly suitable for the extensive parallel preparation in the industrial production, have broad application prospects.
Description of drawings
Fig. 1 is a kind of concrete structure schematic diagram of eccentric multichannel adverse current chromatogram equipment of the present invention;
Fig. 2 is the inlet tube and the fairlead connection diagram of Fig. 1 splitter.
Among the figure:
The 1-casing; 2-fixation hollow axle; 3-splitter hollow shaft; The 4-splitter;
The 5-inlet tube; The 6-fairlead; 7-separates the strand open tubular column; The 8-bearing;
The last plate wheel of 9-; Plate wheel under the 10-; The 11-bearing; The 12-bearing;
The 13-bearing; 14-is hollow shaft initiatively; 15-bearing 16-driving gear;
The 17-fixed gear; The 18-driven gear; The 19-motor; The 20-driving-belt;
The 21-steady brace; The 22-fixed chuck; The 23-fixed chuck; 24-splitter support;
The 25-bearing;
A, B, C-split tunnel group; A 1~A 8The split tunnel of expression A split tunnel group, B 1~B 8The split tunnel of expression B split tunnel group, C 1~C 8The split tunnel of expression C split tunnel group;
(contain A, B, C, A in the text description below the figure neutralization 1~A 8, B 1~B 8, C 1~C 8Mark represent the member relevant with this channel group or passage, all splitters as splitter 4A represents channel group A comprise A 1~A 8, fairlead 6C 1The channel C of expression channel group C 1Fairlead; Do not mark one by one in the accompanying drawings with the label of each split tunnel group and corresponding inlet tube 5 of each split tunnel and fairlead 6).
The specific embodiment
Below by specific embodiment technical scheme of the present invention is further described.
Embodiment 1
Eccentric multichannel adverse current chromatogram equipment shown in Figure 1, comprise casing 1, three groups can around the revolution of fixation hollow axle 2 centers at casing center simultaneously again around splitter hollow shaft 3 synchronously in the same way splitters 4 of rotation (4A, 4B, 4C) and the inlet tube 5 (5A, 5B, 5C) that is connected with splitter and fairlead 6 ((6A, 6B, 6C) is equipped with between the splitter hollow shaft 3 to what prevent inlet tube 5 and 6 dozens of strands of fairlead and twists open tubular column 7 with paired the separating of synchronous reverse rotation of splitter hollow shaft 3.Every group of splitter 4 is made up of eight splitters, and for example A group splitter 4A is by eight splitter 4A 1~4A 8Form the splitter support 24A of these eight splitters 1~24A 83A is distributed on the same circumference around the splitter hollow shaft, thereby forms eccentric multi-channel structure.
Three splitter hollow shafts 3 (3A, 3B, 3C) and three separate strand hollow shaft 7, and (two ends 7C) are installed in up and down on two plate wheels 9,10 by bearing 8,25 respectively for 7A, 7B, and plate wheel 9,10 is linked into an integrated entity by steady brace 21 up and down.The top of fixation hollow axle 2 is installed in the center of plate wheel 9 by bearing 11, and its bottom is bearing on the bearing 13 by the bearing 12 that is installed in down plate wheel 10 centers, and bearing is fixed in the center of casing 1 base plate.Initiatively the bottom of hollow shaft 14 is fixed on plate wheel 9 centers, and the top is installed on the top board of casing 1 by bearing 15.In order to realize synchronously rotation in the same way and revolution, fixed gear 17 equal diameters of installing and being meshing with each other on the driving gear of installing on the declutch shaft hollow shaft 3 16 and the fixation hollow axle 2.Simultaneously for understanding strand, driving gear 16 is with driven gear 18 equal diameters of separating installing on the strand hollow shaft 7 and be meshing with each other.During the instrument operation, the motor 19 that is installed in casing one side drives initiatively by driving-belt 20, and hollow shaft 14 rotates, initiatively hollow shaft 14 and plate wheel 9 up and down, 10 rotate together, thereby the splitter 4 that causes splitter hollow shaft 3 and upward installation thereof revolves round the sun simultaneously again around the 3 center line rotations of splitter hollow shaft around the fixed center shaft centre line synchronously.This motion is for the two-phase liquid in the splitter 4 provides good distributive condition.
Separator tube can be corrosion-resistant pipe such as polyfluortetraethylene pipe, Stainless Steel pipe, can adopt prismatic round tube, rectangle pipe, square, also can adopt inside pipe wall to be the pipe of screw-like or ripple strand shape.The coiling direction of separator tube can be the hand of spiral or coil direction, and its number of plies can be single or multiple lift.Separation tubing string by hand of spiral coiling is spiral tube, is the coiling tubing string by the separation tubing string of coil direction coiling.
The inlet tube of the eccentric multichannel adverse current chromatogram of Fig. 1 device separates post and the parallel in the same way connected mode of fairlead are as shown in Figure 2, the inlet tube 5 (5A, 5B, 5C) of all splitters 4 (4A, 4B, 4C) is at first from being fixed in the fixed chuck 22 parallel fixation hollow axles 2 that penetrate on the casing 1, the Xiang Duan of arrival fixation hollow axle 2 enters the bottom of active hollow shaft 14 and passes from its side perforate, enter the middle and upper part tapping of splitter hollow shaft 3A, wherein splitter 4A (4A by the top of splitter hollow shaft 3A 1~4A 8) inlet tube 5A (5A 1~5A 8), the perforate by splitter hollow shaft 3A middle and upper part respectively with splitter 4A (4A 1~4A 8) leading-in end connect, and splitter 4B, the inlet tube 5B of 4C, 5C continue to walk downwards side by side, the middle and lower part tapping of splitter hollow shaft 3A with respectively with splitter 4A (4A 1~4A 8) the fairlead 6A (6A that links to each other of exit 1~6A 8) compile, the parallel bottom that passes splitter hollow shaft 3A enters and passes from its bottom from the top of separating strand hollow shaft 7A.Parallel inlet tube 5B, 5C and fairlead 6A enter the middle and upper part tapping of splitter hollow shaft 3B, wherein splitter 4B (4B by the top of splitter hollow shaft 3B 1~4B 8) inlet tube 5B (5B 1~5B 8) by splitter hollow shaft 3B middle and upper part perforate respectively with splitter 4B (4B 1~4B 8) leading-in end connect, and the inlet tube 5C of the fairlead 6A of splitter 4A and splitter 4C continues to walk downwards side by side, the middle and lower part tapping of splitter hollow shaft 3B with respectively with splitter 4B (4B 1~4B 8) the fairlead 6B (6B that links to each other of exit 1~6B 8) compile, the parallel bottom that passes splitter hollow shaft 3B enters and passes from its bottom from the top of separating strand hollow shaft 7B.Parallel inlet tube 5C and fairlead 6A, 6B enters the middle and upper part tapping of splitter hollow shaft 3C, wherein splitter 4C (4C by the top of splitter hollow shaft 3C 1~4C 8) inlet tube 5C (5C 1~5C 8) by splitter hollow shaft 3C middle and upper part perforate respectively with splitter 4C (4C 1~4C 8) leading-in end connect, and splitter 4A, the fairlead 6A of 4B, 6B continue to walk downwards side by side, at middle and lower part tapping and the splitter 4C (4C of splitter hollow shaft 3C 1~4C 8) the fairlead 6C (6C that links to each other of exit 1~6C 8) compile, the parallel bottom that passes splitter hollow shaft 3C enters and passes from its bottom from the top of separating strand hollow shaft 7C.Parallel fairlead 6A, 6B, 6C side, the bottom perforate by active hollow shaft 14 enters initiatively hollow shaft 14 and upwards passes, and draws outside the counter-current chromatograph casing by the fixed chuck 23 that is fixed on casing 1 top board.
Adverse current chromatogram equipment shown in Figure 1, its splitter 4A 1~4A 8, 4B 1~4B 8, 4C 1~4C 8Also can adopt the screw type disk post of unitary construction, be convenient to a plurality of screw type disk post of assembling on same splitter hollow shaft 3, to satisfy different chromatographic isolation requirements.

Claims (8)

1. multichannel adverse current chromatogram method of off-centre, it is characterized in that inlet tube is connected according to identical connected mode is parallel in the same way with fairlead with using separately independently with the splitter of splitter hollow shaft decentered distribution more than three or three, make each splitter finish independently chromatographic run.
2. method according to claim 1 and the eccentric multichannel adverse current chromatogram equipment that designs, comprise: casing (1), can be around the revolution of fixation hollow axle (2) center at casing center simultaneously again around splitter hollow shaft (3) the central synchronous splitter of rotation (4) in the same way, and the inlet tube (5) that is connected with splitter, fairlead (6) and with the paired synchronous reverse rotation of splitter hollow shaft (3) separate strand open tubular column (7), it is characterized in that having two or more splitter hollow shafts (3) of symmetrical distribution, each splitter hollow shaft (3) is provided with the splitter (4) of two or more and splitter hollow shaft (3) decentered distribution, and all splitters (4) are by independently inlet tube (5) and fairlead (6) walk abreast in the same way and be connected separately.
3. adverse current chromatogram equipment according to claim 2 is characterized in that said splitter (4) is the spiral tube that is formed according to hand of spiral coiling by separator tube, or the coiling tubing string that is formed according to the coil direction coiling by separator tube.
4. adverse current chromatogram equipment according to claim 3 is characterized in that separator tube is polyfluortetraethylene pipe, stainless steel tube or glass tube.
5. adverse current chromatogram equipment according to claim 3 is characterized in that the cross section of separator tube is circle, rectangle or square.
6. adverse current chromatogram equipment according to claim 3, the inwall that it is characterized in that separator tube is the plane or is screw-like or corrugated.
7. adverse current chromatogram equipment according to claim 2, the preparation capacity that it is characterized in that said splitter (4) are analytic type, half preparation type, preparation type or industrial production type.
8. adverse current chromatogram equipment according to claim 2 is characterized in that being provided with in the casing (1) heating module of controlling separation temperature.
CN2007100681154A 2007-04-17 2007-04-17 Refluent chromatogram method and equipment with eccentric multiple channels Expired - Fee Related CN101091840B (en)

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Application Number Priority Date Filing Date Title
CN2007100681154A CN101091840B (en) 2007-04-17 2007-04-17 Refluent chromatogram method and equipment with eccentric multiple channels

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Application Number Priority Date Filing Date Title
CN2007100681154A CN101091840B (en) 2007-04-17 2007-04-17 Refluent chromatogram method and equipment with eccentric multiple channels

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CN101091840A true CN101091840A (en) 2007-12-26
CN101091840B CN101091840B (en) 2010-07-28

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102192965A (en) * 2010-03-05 2011-09-21 江阴逆流科技有限公司 Eccentric rotating spiral tube separating column device applied to high speed counter current chromatograph
CN102489042A (en) * 2011-12-26 2012-06-13 哈尔滨工业大学 Two-dimensional chromatography multi-channel separating and purifying apparatus and method
CN104226217A (en) * 2013-06-13 2014-12-24 宁波工程学院 Supergravity microtube reactor
CN114222632A (en) * 2019-08-22 2022-03-22 三九股份公司 Separation of particles by centrifugal sedimentation

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102192965A (en) * 2010-03-05 2011-09-21 江阴逆流科技有限公司 Eccentric rotating spiral tube separating column device applied to high speed counter current chromatograph
CN102489042A (en) * 2011-12-26 2012-06-13 哈尔滨工业大学 Two-dimensional chromatography multi-channel separating and purifying apparatus and method
CN102489042B (en) * 2011-12-26 2013-09-04 哈尔滨工业大学 Two-dimensional chromatography multi-channel separating and purifying method
CN104226217A (en) * 2013-06-13 2014-12-24 宁波工程学院 Supergravity microtube reactor
CN104226217B (en) * 2013-06-13 2016-06-01 宁波工程学院 A kind of hypergravity microchannel reactor
CN114222632A (en) * 2019-08-22 2022-03-22 三九股份公司 Separation of particles by centrifugal sedimentation
CN114222632B (en) * 2019-08-22 2024-04-02 格里马尔迪发展有限公司 Separation of particles by centrifugal sedimentation

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