CN1307679A - Device for continuous annular chromatography - Google Patents

Abstract

This invention relates to an apparatus for performing continuous cyclic chromatographic analysis, comprising a columnar shell-shaped particle bed and at least one feeding point for a liquid load. Relative movement occurs between the particle bed and the feeding point. A key feature of this invention is that the lower end of the particle bed cavity is provided with at least one opening (12, 32) facing the particle bed, particularly for conveying the bed material.

Description

Apparatus for performing continuous loop chromatography

The invention relates to a device for performing continuous loop chromatography in which a relative movement is produced between a bed of particles in the shape of a cylindrical shell and at least one feed point of a fluid charge.

In column chromatography, a column is packed with granular material and topped with a mixture of components for isolation. Elution with solvent is then carried out continuously from the top, during which the components are separated according to their different affinities to the particulate material in a ratio proportional to the flow rate of the solvent (eluent) and successively discharged from the column.

One can tell the difference between using a single solvent (principle of constant solvent action) and using multiple different solvents (principle of fractional or gradient action). In the principle of fractional action, the solvent undergoes no transitional changes, whereas in the principle of gradient action, the composition of a solvent in a solvent mixture changes with time.

In eluting chromatography, the components are simply washed through the column; Components with higher affinity and thus replace displacement chromatography using elution chromatography for concentration separation, but this method does not retain all pure single components (always leaves a mixture).

To enable continuous chromatography, circular chromatography was developed, in which a relative movement is created between a columnar bed of particles and a feed point for a liquid charge arranged at least on top of it, a single component in a helical track passing through The granular material is discharged simultaneously on different peripheral areas along the lower part of the cylindrical body periphery. For example, elution or displacement chromatography can be used as HPLC and a constant solution is delivered first.

From this, it can be seen that the difference between the two examples of the rotation of the particle bed relative to the charge and the rotation of the charge relative to the particle bed can be seen. Examples of particle bed rotation are disclosed in eg US-A 5045209 to Westinghouse Electric Company, which describes the chromatographic extraction of scandium and yttrium. References to examples of static particle beds are eg US-A 5149436 to Union Oil Company of California, which describes displacement chromatography for all purposes.

The present invention relates to a circular chromatographic analysis device further developed on the basis of all known technologies, which achieves the purpose of changing the particle bed without dismantling the device.

In order to achieve this object, the device according to the invention is essentially characterized in that at the lower end of the cavity of the particle bed at least one inlet to the particle bed, in particular for discharging the bed material, is provided.

Through said inlet, the bed material can be emptied downwards, preferably by flushing out the old bed material with liquid, so that the device can be refilled with new material from above. Back injection with a high pressure medium such as compressed air is also possible through the inlet in order to break up the particle bed. The unit with bed material enables relative movement between the cavity of the granular bed and the filling point of the new granular bed material, whether emptied or filled with fresh material, the simple way being next to the filling point of the liquid loading material Set up the piping.

Preferred inlets are annular openings, and especially openable openings in which the volume of the hollow sealing means can be varied through the inner space of the opening. A preferred inlet is an inlet formed by a seal that collapses under negative pressure.

It is thus also conceivable that an at least sectionally movable particle bed cavity wall can be provided for forming and closing the inlet.

The present invention will be described in detail below in conjunction with two embodiments associated with the accompanying drawings. Figure 1 and Figure 2 are schematic side sectional views respectively, which show a circular chromatographic analysis device with a static feeding point and a rotating particle bed. Parts corresponding to each other are denoted by the same reference numerals.

A fixed support plate 2 and a movable support arm 3 are arranged on the column 1 . A rotating part 4 driven from the bottom passes through the support plate 2, and the rotating part 4 is supported on the support plate 2 through a tapered roller bearing 5 and fixed on the base 6 with bolts. The middle part of the base 6 has a middle protrusion 7, the protrusion 7 supports a cylindrical hollow part 8 with a conical top 9 . A cylindrical wall 10 concentric with the hollow body 8 is bolted to the base from the top of the base 6, wherein a vertical annular space 11 is left between the hollow body 8 and the cylindrical wall 10, and a vertical annular space 11 is left between the hollow body 8 and the A horizontal plate 12 extending inwards to the middle protrusion 7 is provided between the lower edge and the upper side of the base 6 , and an annular hollow seal 13 is provided on the horizontal plate 12 . A through hole 14 is provided on the base 6 , which communicates the horizontal plate 12 with the underside 15 of the base 6 .

The cylindrical wall 10 supports the cover 16 and the bearing sleeve 17 with the tapered roller bearing 18, which is centrally supported on a fixed feeding unit 19 held by the support arm 3, so that when driven, all mounted on the rotating part Parts on 4 all rotate relative to support plate 12 and feeding unit 19.

The vertical annular space 11 is filled with a granular bed material, typically eg a gel-like material, a separate exchange material (lonentauscher material) or the like, and said material is fed in via a feed unit 19 from the point indicated by reference numeral 20 . Again, the liquid charge is delivered from here and the eluent flows in the middle indicated at 21 to the bed material in chamber 11 via disc meter 22 and cone 9 . At the bottom of the bed of material there is a removable support 23 arranged in a circular shape passing through the bottom plate 6 and the support plate 2 supports a collecting trough 24 for receiving a not shown collector. Reference numeral 25 represents a lateral guide tube.

If the bed material is to be replaced, the hollow seal 13 can be collapsed through the negative pressure tube 26 , thereby opening the opening of the horizontal plate 12 toward the hole 14 and replacing the bed material in the collection tank 24 . Reference numeral 27 denotes a ventilation or compressed air line by means of which the hollow seal 13 can be decompressed during operation of the device.

Compared with the device shown in FIG. 1 , the device shown in FIG. 2 omits the seal that can open and close the annular cavity and has a variable volume, but under the action of the hydraulic or pneumatic cylinder piston assembly 28,29 The entire hollow part 8 is lifted from the base 6, and the piston assembly is supported on the middle raised part 7 of the base through a bracket 30. As a result, the lower annular periphery 31 of the hollow part 8 , which is secured in the groove in a stationary, sealed state, can be lifted out of the corresponding annular groove 32 of the base 6 . A through hole 14 is provided at the bottom of the annular groove 32 . Apart from this, the embodiments of FIGS. 1 and 2 and their operation correspond.

Claims (5)

1. be used to carry out the device of continuous circular shape stratographic analysis, wherein between at least one feeding point of the grain bed of cylindrical wall form and liquid loaded stock, form relative motion, it is characterized in that, the lower end of grain bed cavity (11) is provided with at least one inlet (12,32) of carrying especially for the bed material towards grain bed.

2. device according to claim 1 is characterized in that, inlet (12,32) is an annular opening.

3. device according to claim 1 and 2 is characterized in that, is provided with a hollow closure means (13) that can change its volume by internal cavities in inlet (12).

4. device according to claim 3 is characterized in that, packoff (13) produces under the effect of negative pressure equipment and subsides.

5. device according to claim 1 and 2 is characterized in that, the wall (8) of grain bed cavity (11) sectional at least moves.

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