CN101042384B

CN101042384B - Conicity counterflow chromatograph

Info

Publication number: CN101042384B
Application number: CN200710068114A
Authority: CN
Inventors: 吴世华
Original assignee: Zhejiang University ZJU
Current assignee: Zhejiang University ZJU
Priority date: 2007-04-17
Filing date: 2007-04-17
Publication date: 2010-05-26
Anticipated expiration: 2027-04-17
Also published as: CN101042384A

Abstract

This invention relates to one tamper inverse chromatographic apparatus, which comprises case body; isolation column rolling around its axis with more than one rolling case center fix hollow axis center; separation column lead tube, lead out tube and de-crush hollow column to avoid lead in and out tube and separation hollow axis. The invention is characterized by the separation column composed of separation column racks from left to right directions on tamper surface.

Description

Conicity counterflow chromatograph

Technical field

The present invention relates to the adverse current chromatogram separation field, relate to the adverse current chromatogram equipment 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 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 up to the present, the separating column support of all kinds of high-speed counter-current chromatographs is right cylinder.The helix tube type separating column of this face of cylinder coiling, its centrifugal force field is for being plane distribution, radial force that two-phase fluid is subjected to and tangential force gradient are zero, although can realize the one-way of two-phase fluid distributes, but its equilibration time is longer relatively, the stationary phase retention is relatively low, and usually forms bubble in separating tubing string.

People such as Y.ITO (United States Patent (USP) 6,379,973 (2002); J.Liq.Chromatogr.Rel.Technol.26 (2003) 1355; Journal of Chromatography A, 1017 (2003) 71-81) and Chinese patent ZL02250372.2 reported several scroll disk pillar high speed adverse current chromatograms, increased the radial gradient of centrifugal force field, some shortcomings of existing high speed adverse current chromatogram have been improved, but these method and apparatus but can not strengthen the tangential gradient of its centrifugal force field, and its coiling pipeline complexity, also the connection tube seat must be arranged between each folded dish, reduce the space utilization degree of instrument, unfavorablely used industrialized production.

Summary of the invention

The objective of the invention is to overcome the deficiency of present above-mentioned adverse current chromatogram equipment, and a kind of radial force field gradient that can strengthen existing high speed adverse current chromatogram is provided, can strengthen the conicity counterflow chromatograph of its tangential force field gradient again.

Conicity counterflow chromatograph of the present invention comprises casing, one or more 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 separating column is wound on the separating column support that the surface is the conical surface according to left hand direction or dextrorotation direction by separator tube to constitute.

Among the present invention, the tapering of the conical surface of said separating column support is the unspecified angle in 5-87 °.For the ease of processing and provide the centrifugal force field of optimization, the tapering of the conical surface of preferable separate column holder is 5 °, 9 °, and 15 °, 20 °, 28 °, 34 ° or 40 °.

Among the present invention, said separator tube can be polyfluortetraethylene pipe, stainless-steel tube or glass tube.The cross section of separator tube is circle, rectangle or square.The inwall of separator tube can be the plane or be screw-like or corrugated.

Among the present invention, the separator tube coiling number of plies that constitutes separating column can be a single or multiple lift, and the preparation capacity of 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:

This separation tubing string that is conical surface coiling, the radial centrifugal force field and tangential centrifugal force field gradient of having strengthened the contrary chromatogram of existing high speed, disengaging time has been shortened in the reservation that has improved stationary phase, has increased separation efficiency.And the coiling of separator tube also is easy to carry out, and the space utilization degree of separating column is also very high, is particularly suitable for the separation of biological sample.

Description of drawings

Fig. 1 is a kind of concrete structure synoptic diagram of conicity counterflow chromatograph of the present invention;

Fig. 2 is the connection diagram of the inlet tube and the fairlead of Fig. 1 separating column.

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; A, B, the C-split tunnel (contain A in the text description below the figure neutralization, B, the mark of C is represented the member relevant with this passage, represents the separating column of A channel as separating column 4A, fairlead 6C represents the fairlead of C-channel;

Separating column

4A, 4B, 4C and with the corresponding inlet tube 5A of separating column, 5B, 5C and fairlead 6A, 6B, the label of 6C 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

Counter-current chromatograph shown in Figure 1, comprise casing 1, three can around fixation hollow axle 2 revolution at casing center simultaneously again around separating column tubular shaft 3 synchronously in the same way the separating columns 4 of rotation (4A, 4B, 4C), and the inlet tube 5 (5A that are connected with separating column, 5B, 5C), fairlead 6 (6A, 6B, 6C), 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 surface is installed on the separating column tubular shaft 3 with one heart for the separating column support 24 of the conical

surface.Separating column

4A, 4B, 4C directly are wound on by left hand direction or dextrorotation direction on the conical surface of separating column support 24 with separator tube respectively and constitute, and its number of plies can be single or multiple lift.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 8,25 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.

The separator tube of 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 inlet tube 5 of each separating column 4 of Fig. 1 counter-current chromatograph and fairlead 6 can adopt to walk abreast and be connected to form multichannel adverse current chromatogram, also can be connected in series successively, and form single pass adverse current chromatogram.

With parallel connected mode shown in Figure 2 is example, three parallel separating column 4A that connect have been adopted, 4B, 4C, separating

column

4A, 4B, the inlet tube 5A of 4C, 5B, 5C 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 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 the inlet tube 5A of separating column 4A by separating column tubular shaft 3A middle and upper part passes and is connected with the leading-in end of separating column 4A, and the inlet tube 5B of separating

column

4B and 4C and 5C continue to walk downwards side by side, the fairlead 6A that links to each other with exit with separating column 4A at the middle and lower part tapping of separating column tubular shaft 3A compiles, and 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, 5C and fairlead 6A enter the middle and upper part tapping of separating column tubular shaft 3B by the top of separating column tubular shaft 3B, wherein the inlet tube 5B of separating column 4B passes by the perforate of separating column tubular shaft 3B middle and upper part, be connected with the leading-in end of separating column 4B, and the inlet tube 6C of the fairlead 6A of separating column 4A and separating column 4C continues to walk downwards side by side, middle and lower part tapping at separating column tubular shaft 3B compiles with the fairlead 6B that the exit of separating column 4B links to each other, the parallel bottom that passes separating column tubular shaft 3B enters and passes from its bottom from the top of separating strand tubular shaft 7B.Parallel inlet tube 5C and fairlead 6A, 6B enters the middle and upper part tapping of separating column tubular shaft 3C by the top of separating column tubular shaft 3C, wherein the inlet tube 6C of separating column 4C passes by the perforate of separating column tubular shaft 3C middle and upper part, be connected with the leading-in end of separating column 4C, and the fairlead 6A of separating

column

4A and 4B, 6B continues to walk downwards side by side, middle and lower part tapping at separating column tubular shaft 3C compiles with the fairlead 6C that the exit of separating column 4C links to each other, the parallel bottom that passes separating column tubular shaft 3C enters and passes from its bottom from the top of separating strand tubular shaft 7C.Parallel fairlead 6A, 6B 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.

Counter-current chromatograph shown in Figure 1, the cone angle of the conical surface of separating column support 24 are the 5-87 degree.For the ease of processing and provide the centrifugal force field of optimization, the cone angle of the conical surface of preferable separate column holder is 5 °, 9 °, and 15 °, 20 °, 28 °, 34 °, 40 °.

Counter-current chromatograph shown in Figure 1, on every separating column tubular shaft 3, can install the separating column that (is designated as n) more than, the inlet tube of each separating column is connected according to the connected mode identical with Fig. 2 is parallel respectively in the same way with fairlead, thereby forms 3n chromatographic resolution passage.

Claims

1. conicity counterflow chromatograph, comprise casing (1), one or more 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 twist open column (7) with paired the separating of synchronous reverse rotation of separating column tubular shaft (3), it is characterized in that separating column (4) is wound on the separating column support (24) that the surface is the conical surface according to left hand direction or dextrorotation direction by separator tube to constitute.

2. conicity counterflow chromatograph according to claim 1, the cone angle that it is characterized in that the conical surface of separating column support (24) are the unspecified angle in 5-87 °.

3. conicity counterflow chromatograph according to claim 1, the cone angle that it is characterized in that the conical surface of separating column support (24) is 5 °, 9 °, 15 °, 20 °, 28 °, 34 ° or 40 °.

4. conicity counterflow chromatograph according to claim 1 is characterized in that separator tube is polyfluortetraethylene pipe, stainless-steel tube or glass tube.

5. conicity counterflow chromatograph according to claim 1 is characterized in that the cross section of separator tube is circle, rectangle or square.

6. according to the conicity counterflow chromatograph of claim 1, the inwall that it is characterized in that separator tube is the plane or is screw-like or corrugated.

7. conicity counterflow chromatograph according to claim 1, the separator tube coiling number of plies that it is characterized in that constituting separating column (4) is a single or multiple lift.

8. conicity counterflow chromatograph according to claim 1, the preparation capacity that it is characterized in that separating column (4) are analytic type, half preparation type, preparation type or commercial production type.

9. conicity counterflow chromatograph according to claim 1 is characterized in that being provided with in the casing (1) heating module of controlling separation temperature.