CN101042386A - Bidirectional adverse current chromatograph Method and apparatus thereof - Google Patents
Bidirectional adverse current chromatograph Method and apparatus thereof Download PDFInfo
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- CN101042386A CN101042386A CN 200710068117 CN200710068117A CN101042386A CN 101042386 A CN101042386 A CN 101042386A CN 200710068117 CN200710068117 CN 200710068117 CN 200710068117 A CN200710068117 A CN 200710068117A CN 101042386 A CN101042386 A CN 101042386A
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- adverse current
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Abstract
This invention discloses one double inverse flow color spectrum method and device, which comprises the following steps: using symmetric distributed more than three series separation columns; leading from first one into first phase flow and leading second and leading from second with materials; leading from last separation column end into first phase flow. The device comprises fix hollow center rolling case center and the separation column rolling around axis, leading tube, leading out tube and the de-cross hollow column.
Description
Technical field
The present invention relates to the adverse current chromatogram separation field, relate to a kind of liquid that does not have a solid-state carrier-method of the adverse current chromatogram that the liquid two phase countercurrent flow distributes and the equipment designed specifically according to this method.
Background technology
Adverse current chromatogram is a kind of liquid liquid distribution chromatography without solid-state carrier.Owing to its no irreversible adsorption, 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, spiral pipe is coaxially on supporter, under the effect of its special centrifugal force field, forming unidirectional two-phase distributes, thereby realize the high retention of stationary 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 high capacity and all obtained great application.But present widely used counter-current chromatograph adopts one in the immiscible two-phase as stationary phase mostly, and another carries out the mode of wash-out as mobile phase.This type of elution of having only a phase solvent to flow all will intermittently change stationary phase after the operation each time, so the productive rate of unit interval is not high, and operation is also very loaded down with trivial details.
Y.W.Lee etc. (Journal of liquid chromatography, 1988,11,37-53) reported a kind of mobile method of carrying out the bidirectional adverse current chromatography eluant of high speed adverse current chromatogram realization two-phase solvent of using.Y.ITO (international monopoly WO2004/094985 A3) discloses a kind of application disc realizes the bidirectional adverse current chromatography eluant around spiral tube method.But these two kinds of methods all are to adopt single separating column structure, are being provided with on the sun wheel of single separating column and will just can finishing the static equilibrium state with corresponding counterweight.When different solvents and separated object entered separating column, this balance was broken, and can influence the operate as normal of instrument.
Chinese patent ZL00207386.2 " many separating columns high-speed counter-current chromatograph " discloses the different many separating columns counter-current chromatograph of several structures respectively with ZL02261047.2 " high-speed counter-current chromatograph ".These counter-current chromatographs all adopt the same structure of a plurality of series connection and the separating column of same capability, although improved the balance quality of instrument greatly, have increased the preparative capacibility of unit, but can not realize two-way adverse current chromatogram wash-out.
Summary of the invention
The objective of the invention is to overcome the deficiency of present above-mentioned adverse current chromatogram, and a kind of new bidirectional adverse current chromatographic process and equipment are provided.
Bidirectional adverse current chromatographic process of the present invention, it is characterized in that utilizing the separating column that is connected in series more than three or three of symmetrical distribution to carry out the bidirectional adverse current chromatographic resolution, introduce first phase fluid and draw second phase fluid from the head end of first separating column, introduce second phase fluid and draw first phase fluid from the tail end of last separating column, introduce material to be separated from second separating column.
The bidirectional adverse current chromatographic equipment that adopts said method and design, comprise casing, can be around the revolution of the fixation hollow axle center at casing center simultaneously again around the separating column tubular shaft central synchronous separating column of rotation in the same way, and the inlet tube that is connected with separating column, fairlead and with the paired synchronous reverse rotation of separating column tubular shaft separate the strand open column, it is characterized in that said separating column has more than three or three, each separating column is connected with a pipeline connector at least, the separating column that is connected with pipeline connector is connected in series by connecting pipe successively, inlet tube links to each other with an arm of pipeline connector, and fairlead links to each other with another arm of pipeline connector.
Among the present invention, said separating column can be 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.Separator tube can adopt 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 be the plane or be screw-like or corrugated.
Among the present invention, the preparation capacity of said separating column is analytic type, half preparation type, preparation type or commercial production type.Usually, in casing, be provided with the heating module of control separation temperature.
Beneficial effect of the present invention is:
The present invention adopts the separating column that is connected in series more than three or three to carry out the bidirectional adverse current chromatographic resolution, the needs that adapt to continuous high-efficient bidirectional adverse current wash-out, not only improved the balanced capacity of instrument, and improved the preparative capacibility of unit, improve the production efficiency of unit interval greatly, reduced operating cost, be particularly suitable for the large scale analysis and the preparation of biological sample, be particularly suitable for the mass preparation in the commercial production, have broad application prospects.
Description of drawings
Fig. 1 is a concrete structure synoptic diagram of the present invention;
Fig. 2 is the separating column of the equipment shown in Figure 1 synoptic diagram that is connected in series;
Fig. 3 is the synoptic diagram that separating column was introduced and drawn to Fig. 1 two-phase fluid and sample introduction material.
Among the figure:
The 1-casing; 2-fixation hollow axle; 3-separating column tubular shaft; The 4-separating column;
The 5-inlet tube; The 6-fairlead; 7-separates the strand open 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 tubular shaft initiatively; The 15-bearing; The 16-driving gear;
The 17-fixed gear; The 18-follower gear; The 19-motor; The 20-driving-belt;
The 21-steady brace; The 22-fixed chuck; The 23-fixed chuck; 24-separating column support;
The 25-bearing; The 26-pipeline connector; 27-top arm; The 28-side branch;
Arm at the bottom of the 29-; The 30-connecting pipe;
A, B, C ,-separating column (contain A in the text description below the figure neutralization, B, the mark of C is represented the member relevant with this separating column, represents separating column A as 4A, and 5A represents to separate the inlet tube of tubing string 4A, and 30B represents the connecting pipe that links to each other with separating column 4B; Separating column 4A, 4B, 4C and with the corresponding inlet tube 5A of separating column, 5B, 5C, fairlead 6A, 6C and connecting pipe 30A, 30B and pipeline connector 26A, 26B, the label of 26C in the accompanying drawings one by one the mark).
Embodiment
Below by specific embodiment technical scheme of the present invention is further described.
Embodiment 1
Bidirectional adverse current chromatographic equipment shown in Figure 1, comprise casing 1, three can be around the revolution of fixation hollow axle 2 centers at casing center simultaneously again around the separating column tubular shaft 3 central synchronous separating column 4 (4A of rotation in the same way, 4B, 4C), and the inlet tube 5, the fairlead 6 that are connected with separating column 4, this example, each separating column 4 is connected with a pipeline connector 26, three separating columns 4 are connected in series by the end arm 29 and the connecting pipe 30 of pipeline connector successively, the top arm 27 of pipeline connector links to each other with inlet tube 5, the side branch 28 of the pipeline connector (see figure 3) that links to each other with fairlead 6.Three separating column 4A, 4B, 4C directly are wound on by identical mode on the separating column support 24 of separating column tubular shaft 3 with separator tube respectively and constitute.Be equipped with between the separating column tubular shaft 3 for prevent inlet tube 5 and 6 dozens of strands of fairlead with the paired synchronous reverse rotation of separating column tubular shaft 3 separate strand open column 7.The two ends that separating column tubular shaft 3 is conciliate strand tubular shafts 7 are installed in up and down on two plate wheels 9,10 by bearing 8 and bearing 25 respectively, 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 tubular 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 separating column tubular shaft 3 16 and the fixation hollow axle 2.Simultaneously for understanding strand, driving gear 16 is with follower gear 18 equal diameters of separating installing on the strand tubular 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 tubular shaft 14 rotates, initiatively tubular shaft 14 and plate wheel 9 up and down, 10 rotate together, thereby the separating column 4 that is installed on the separating column tubular shaft 3 is revolved round the sun simultaneously again around the 3 center line rotations of separating column tubular shaft around fixation hollow axle 2 centers synchronously.This motion is for the two-phase liquid in the separating column 4 provides good distributive condition.
Three separating column 4A, 4B, 4C are connected in series as Fig. 2, shown in Figure 3.Three separating column 4A, 4B, the inlet tube 5A of 4C, 5B, 5C, at first from being fixed in fixation hollow axle 2 parallel the penetrating on the casing 1, the top of arrival fixation hollow axle 2 enters the bottom of active tubular shaft 14 and passes from its side perforate, enter the middle and upper part tapping of separating column tubular shaft 3A by the top of separating column tubular shaft 3A, wherein the perforate of inlet tube 5A by separating column tubular shaft 3A middle and upper part pass be connected with the top arm 27A of pipeline connector 26A and by the road connector 26A insert certain-length in the leading-in end of separator tube of the separating column 4A that is connected with the end arm 29A of pipeline connector 26A, the perforate that the side branch 28A of pipeline connector 26A is connected with the fairlead 6A that draws second phase fluid by separating column tubular shaft 3A middle and upper part enters in the separating column tubular shaft 3A, and with inlet tube 5B, 5C together walks downwards side by side, middle and lower part tapping at separating column tubular shaft 3A compiles with the connecting pipe 30A that the exit of separating column 4A links to each other, the parallel bottom that passes separating column tubular shaft 3A enters and passes from its bottom from the top of separating strand tubular shaft 7A. Parallel inlet tube 5B and 5C and fairlead 6A and connecting pipe 30A enter the middle and upper part of separating column tubular shaft 3B by the top of separating column tubular shaft 3B, inlet tube 5B and the connecting pipe 30A perforate by separating column tubular shaft 3A middle and upper part passes respectively and is connected with side branch 28B with the top arm 27B of pipeline connector 26B, wherein inlet tube 5B by the road connector 26B insert certain-length in the separator tube of the separating column 4B be connected with the end arm 29B of pipeline connector 26B, and inlet tube 5C and fairlead 6A continue along separating column tubular shaft 3B is parallel to walk downwards, middle and lower part tapping at separating column tubular shaft 3B compiles with the connecting pipe 30B that the exit of separating column 4B links to each other, the parallel bottom that passes separating column tubular shaft 3A enters and passes from its bottom from the top of separating strand tubular shaft 7A.Parallel inlet tube 5C and fairlead 6A and connecting pipe 30B enter the middle and upper part of separating column tubular shaft 3C by the top of separating column tubular shaft 3C, the perforate of connecting pipe 30B by separating column tubular shaft 3C middle and upper part passes with the leading-in end of separating column 4C and is connected, and inlet tube 5C and fairlead 6A continue to walk downwards side by side, arrive the middle and lower part of separating column tubular shaft 3C, the perforate of the inlet tube 5C that wherein introduces second phase fluid by separating column tubular shaft 3C middle and lower part pass be connected with the top arm 27C of pipeline connector 26C and by the road connector 26C insert certain-length in the separator tube of the separating column 4C that is connected with arm 29C at the bottom of the pipeline connector 26C, and the side branch 28C of pipeline connector 26C is connected with the fairlead 6C that draws first phase fluid and the perforate through separating column tubular shaft 3C middle and lower part penetrates, with the parallel bottom that passes separating column tubular shaft 3C of fairlead 6A, enter and pass from its bottom from the top of separating strand tubular shaft 7C.Parallel fairlead 6A and 6C side, the bottom perforate by active tubular shaft 14 enters initiatively tubular 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.
Fig. 3 shows the flow graph of two-phase fluid and sample introduction material.First phase fluid connector 26A is by the road introduced and is drawn from the tail end of last separating column 4C from the head end of first separating column 4A, second phase fluid connector 26C is by the road introduced and is drawn from the head end of first separating column 4A from the tail end of last separating column 4C, and sample introduction material connector 26B is by the road introduced from second separating column 4B.
The separator tube of coiling separating column 4 can be corrosion-resistant pipe such as polyfluortetraethylene pipe, stainless-steel tube or glass tube.Separator tube can adopt round tube, rectangle pipe or square tube, and the inwall of separator tube can be the plane or is screw-like or undulatory pipe.
The coiling direction of separator tube can be the hand of spiral or coil direction.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.According to diameter, length and the pipe capacity of coiling pipeline, separating column 4 can be analytic type, partly preparation property, preparation property and commercial production type.
Claims (8)
1. bidirectional adverse current chromatographic process, it is characterized in that utilizing the separating column that is connected in series more than three or three of symmetrical distribution to carry out the bidirectional adverse current chromatographic resolution, introduce first phase fluid and draw second phase fluid from the head end of first separating column, introduce second phase fluid and draw first phase fluid from the tail end of last separating column, introduce material to be separated from second separating column.
2. method according to claim 1 and the bidirectional adverse current chromatographic equipment that designs, comprise casing (1), can be around the revolution of fixation hollow axle (2) center at casing center simultaneously again around separating column tubular shaft (3) the central synchronous separating column of rotation (4) in the same way, and the inlet tube (5) that is connected with separating column (4), fairlead (6) and with the paired synchronous reverse rotation of separating column tubular shaft (3) separate strand open column (7), it is characterized in that: said separating column (4) has more than three or three, each separating column (4) is connected with a pipeline connector (26) at least, the separating column (4) that is connected with pipeline connector (26) is connected in series by connecting pipe (30) successively, inlet tube (5) links to each other with an arm (27) of pipeline connector, and fairlead (6) links to each other with another arm (28) of pipeline connector.
3. adverse current chromatogram equipment according to claim 2 is characterized in that said separating column (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 separating column (4) are analytic type, half preparation type, preparation type or commercial 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.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200710068117 CN101042386A (en) | 2007-04-17 | 2007-04-17 | Bidirectional adverse current chromatograph Method and apparatus thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200710068117 CN101042386A (en) | 2007-04-17 | 2007-04-17 | Bidirectional adverse current chromatograph Method and apparatus thereof |
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| Publication Number | Publication Date |
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| CN101042386A true CN101042386A (en) | 2007-09-26 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN 200710068117 Pending CN101042386A (en) | 2007-04-17 | 2007-04-17 | Bidirectional adverse current chromatograph Method and apparatus thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101676716A (en) * | 2008-09-16 | 2010-03-24 | 江阴逆流科技有限公司 | Inlet pipe and outlet pipe concurrent and circumambulated device applied in multi-column counter current chromatograph |
-
2007
- 2007-04-17 CN CN 200710068117 patent/CN101042386A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101676716A (en) * | 2008-09-16 | 2010-03-24 | 江阴逆流科技有限公司 | Inlet pipe and outlet pipe concurrent and circumambulated device applied in multi-column counter current chromatograph |
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Open date: 20070926 |