JPH08145973A - Apparatus and method for filling resin of circular chromatograph - Google Patents

Abstract

PURPOSE: To uniformly fill by preventing the precipitation of resin during filling of the resin to be filled. CONSTITUTION: The apparatus for filling the resin of a circular chromatograph comprises a porous plate 2 for vertically moving an air gap 1 between an outer cylinder 17 and an inner cylinder 18, an elevating mechanism 3 supporting the plate 2 by the lower ends of a plurality of support rods 4 to vertically move the gap 1, a resin pouring tube 7 for introducing resin slurry 6 to the upper part of the plate 2 upon falling of the plate 2, a pouring tube support arm 9 for coupling the tube 7 to a central rotary shaft 8 to rotate together with the shaft 8, and a consolidating mechanism (not shown) for consolidating the slurry 6 filled in the gap via the plate 2 to form a filled resin layer 16. The resin can be uniformly filled in the narrow gap, the plate is raised to remove the filled resin by one step, and the mixture of refuse, various bacteria, etc., is suppressed to the minimum limit.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an apparatus for separating and purifying a useful substance from a bulk produced in a production process of various useful substances related to biochemistry, and particularly to uniformly filling a separated packed bed with a resin. The present invention relates to a resin filling device and a resin filling method for a circular ring chromatography device suitable for the above.

[0002]

2. Description of the Related Art With the progress of biotechnology, various useful substances related to biochemistry have been produced on an industrial scale. In the production process of these useful substances, the step of separating the target useful substance from the generated bulk and purifying it into a product, that is, a downstream process is important. Although there are various separation means for separating the intended useful substance from the generated bulk, the annular liquid chromatography device is one of the most useful means of handling biochemical-related substances such as pharmaceuticals, foods and dyes. Widely used in such fields.

Regarding the characteristics of the separation by the annular liquid chromatography device, for example, "continuous separation by an annular chromatography device having a rotating inlet and outlet" (Conti)
−nuous separation using an annular chromatog
raph with rotating inlet and outlet; Goto,
S. Goto, J. Chem. Eng. Jap. , 20, 6, 59
9, 1987), targeting separation components such as alcohols, amino acids, salts and saccharides (eg pH, feed rate, ratio of eluent and rotation speed), moment method, mass balance, etc. Engineering studies using models are being conducted.

FIG. 4 shows an example of a conventional single-layer annular liquid chromatography device. An inner cylinder 18 having a space 1 for accommodating the filled resin layer 16 in the inner circumference of the outer cylinder 17, a space 1a sealed inside, and a raw material liquid nozzle 40 for supplying a sample to be separated while rotating into the space 1. An eluent inlet nozzle 41 for supplying an eluent to the void 1, a constant temperature liquid inlet nozzle 42 for feeding and discharging a fluid for holding the filling resin layer 16 at a predetermined temperature in the space 1a, and a filling resin disposed below the void 1 A plurality of separation liquid buckets 43 that collect the separated liquid that has passed through the layer 16, and a rotation drive mechanism 45 that rotates the separation liquid bucket 43 via the central rotation shaft 8 in synchronization with the raw material liquid nozzle 40. A collection tank 46 for collecting the separated concentrated component via the groove 44, and is composed of a raw material supply system, an annular resin packed column system and a separated concentrated component collecting system. In this example, inner diameter 500φ, height 2006mm
The outer cylinder has a built-in inner cylinder having an outer diameter of 480φ and a height of 1840 mm. The thickness of the filled resin layer is 10 mm. In the multi-layered annular liquid chromatography device having a plurality of separated packed beds, the column chromatography device performs the separation by the batch operation, while the continuous supply of raw materials, the separation, and the concentration operation are possible. The feature is that the Japanese Patent Application No. 5-
It is disclosed in Japanese Patent Publication No. 70083 and Japanese Patent Application No. 5-70084. Further, it is disclosed in Japanese Patent Application Laid-Open No. 2-189458 and Japanese Utility Model Laid-Open No. 64-46749, but neither of them describes a method and apparatus for filling a resin in a column.

The chromatographic separation performance is greatly affected by the resin filling condition. In order to uniformly fill the filled resin layer with the resin, it is first necessary to prepare a resin slurry that is uniformly dispersed. For this, a 7: 5 mixture of 1,1,2,2-tetrabromoethane and tetrachloroethylene (Permaphase ETH)
There is an example of using a mixture of water and ethanol (fine particles of all-pores silica) or thin aqueous ammonia, but it is important that the resin does not precipitate during filling. In particular, measures to prevent the precipitation of resin during the filling operation when the column height is high in a large-scale device are a subject for study.

[0006]

In the conventional resin packing device for a ring chromatographic device, a structure for uniformly packing the resin in the packed resin layer of the ring chromatographic device has not been realized.
There is a problem that it is necessary to consider a measure to prevent precipitation during the filling operation when the column height is large in a large-scale device.

An object of the present invention is to provide a resin filling device and a resin filling method for a ring chromatography apparatus capable of preventing the precipitation of the resin during the filling operation of the filled resin layer and uniformly filling the resin.

[0008]

In order to achieve the above-mentioned object, a resin filling device for a ring chromatography device according to the present invention is
A porous plate that can freely move up and down the space between the outer cylinder and the inner cylinder, an elevating mechanism that supports the porous plate at the lower end and moves it up and down in the space, and injects resin slurry into the upper part of the porous plate as the porous plate descends. Consists of a resin injection pipe, an injection pipe support arm that rotates the resin injection pipe by connecting it to the central rotating shaft, and a consolidating mechanism that consolidates the resin slurry filled in the voids through the perforated plate to form a filled resin layer. And

In the resin filling method for the circular ring chromatograph, the porous plate is lowered into the space between the outer cylinder and the inner cylinder,
As it descends, resin slurry is injected into the upper part of the perforated plate via the resin injection pipe, and the resin injection pipe rotates together with the central rotating shaft, and the resin slurry filled in the voids via the perforated plate is compacted and filled. The resin layer is formed, and the porous plate is raised to take out the filled resin layer.

[0010]

According to the present invention, a perforated plate which can be moved up and down by an elevating mechanism is inserted into the space between the outer cylinder and the inner cylinder of the annular chromatograph, and the upper part of the perforated plate is lowered as the perforated plate descends. Since the resin slurry is filled while being introduced, the resin slurry is uniformly filled in the gap between the outer cylinder and the inner cylinder that is long in the axial direction through the perforated plate, and the resin slurry is added by the consolidation mechanism. The filling resin layer is formed by pressing and consolidating. Further, the elevating mechanism raises the perforated plate so that the filled resin layer can be easily taken out in one step. Also, because there are few disassembled parts,
Contaminants such as dust and germs are minimized.

[0011]

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS An embodiment of the present invention will be described with reference to FIGS. As shown in FIGS. 1 to 3, a porous plate 2 capable of moving up and down in a space 1 between an outer cylinder 17 and an inner cylinder 18, and a porous plate 2
And a resin injection pipe 7 for introducing the resin slurry 6 into the upper part of the perforated plate 2 as the perforated plate 2 is lowered, and a resin injection pipe 7 An injection pipe support arm 9 for connecting the central axis of rotation 8 driven by the rotary drive mechanism 45 and rotating the central axis of rotation 8 together with the central axis of rotation 8.
It is configured by a compaction mechanism 30 that compacts the resin slurry 6 filled in the voids 1 via the porous plate 2 to form the filled resin layer 16.

The elevating mechanism 3 includes an elevating groove 17a formed vertically on the inner wall surface of the outer cylinder 17, an elevating groove 18a formed vertically on the outer wall surface of the inner cylinder 18, and an elevating groove. Convex portions (not shown) formed on the perforated plate 2 that can be inserted into 17a and 18a, a support rod elevating arm 10 that fixes the upper ends of the support rods 4, and a wire whose one end is fixed to the approximate center of the support rod elevating arm 10. 11, a plurality of guides 12 that guide the wire 11 so as to be able to move up and down, a planar rack 13 fixed to the other end of the wire 11, a gear 14 that meshes with the rack 13, and a drive mechanism 15 for the gear 14. The resin injection pipe 7 includes a filled resin slurry storage tank 20 having a paddle 22 that is stirred by a stirring motor 21 and a slurry transfer pipe 2.
And a slurry transfer pump 23 for transferring the resin slurry 6 via the nozzle 4. The compaction mechanism 30 is fixed to an annular compaction plate 31 which is crimped onto the upper surface 16 a of the filled resin layer 16, and one end of which is fixed to the upper surface of the compaction plate 31 and the other end of which is fixed to a ring 32 which is inserted through the central rotation shaft 8. A compression plate support arm 33, a lower end of which is fixed to the upper end of the ring 32 and which inserts the central rotary shaft 8 into the compression operation support pipe 35; and a hydraulic jack 34 in which a cylinder is fixed to the upper end of the compression operation support pipe 35. I shall. As shown in FIG. 2, the consolidation plate 31 is detachably attached to the lower surface of a flange 36 provided on the inner cylinder 18 side of the support rod 4, and the hydraulic jack 34 is provided between the flange 36 and the consolidation plate 31. It is also possible to apply various structures, such as mounting and pressing the consolidation plate 31 against the upper surface 16a of the resin slurry. The perforated plate is formed so that the pore diameter and the number of pores are determined according to the properties of the resin slurry to suppress the sedimentation speed of the resin slurry during the filling operation and prevent the resin slurry from settling on the bottom surface of the voids and making it non-uniform. There is a need to.

Next, the operation of this embodiment will be described. The lid 47 of the annular chromatography apparatus shown in FIG. 4 is opened by removing the surrounding fastening bolts, and the convex portions of the perforated plate 2 are lifted and lowered on the inner wall surface of the outer cylinder 17 and the outer wall surface of the inner cylinder 18. Groove 17
The rack 1 that is inserted into the gears a and 18a, drives the drive mechanism 15 to rotate the gear 14 of the lifting mechanism 3, and meshes with the gear 14.
3 is moved upward, and the porous plate 2 is moved up and down while the resin slurry loaded from the resin injection pipe 7 is entrained.
It descends along 18a. The descending speed is balanced with the slurry injection amount so that the upper surface 16a of the injected resin is always equal to the height of the inner cylinder 17. Resin injection pipe 7
Is directly connected to the central rotation shaft 8 via the injection pipe support arm 9, so that the resin slurry is injected while rotating together with the central rotation shaft 8. As for the consolidation of the filling resin, as shown in FIG. 3, a compaction plate 31 driven by a hydraulic jack 34 is installed on the filling resin, and is hydraulically lowered through a consolidation plate support arm 33 to consolidate the resin to fill the filling resin layer 16 To form.

When the filled resin layer 16 is taken out, the resin injection pipe 7, the injection pipe support arm 9 and the raw material liquid nozzle 40 shown in FIG. 4 are removed, and the gear 14 of the lifting mechanism 3 is driven by the drive mechanism 15 to rotate in the reverse direction. Then, the rack 13 that meshes with the gear 14 is moved downward, and the porous plate 2 is pulled up to the upper surface of the inner cylinder 18 via the wire 11 and the support rod 4, so that the filled resin layer 16 can be taken out.

As another embodiment of the present invention, a resin filling method for a ring chromatography device will be described. As described above, the perforated plate 2 and the elevating mechanism 3 are installed in the circular chromatograph, and the elevating mechanism 3 lowers the perforated plate 2 into the space 1 between the outer cylinder 17 and the inner cylinder 18. Resin injection pipe 7 on top of plate 2
The resin slurry 6 is injected through the resin injection pipe 6, the resin injection pipe 6 is rotated together with the central rotating shaft 8, and the resin slurry filled in the voids 1 via the porous plate 2 is consolidated by the consolidation mechanism 30 to fill the resin layer 16 When the filled resin layer 16 is taken out, the porous plate 2 is raised to the upper surface of the inner cylinder 18 by the elevating mechanism 3 and taken out in one step.

According to the present invention, the resin can be uniformly filled in the space between the narrow outer cylinder and the inner cylinder which is long in the axial direction in the ring chromatography apparatus, and the resin is pressurized and compacted to form the filled resin layer. can do. Further, the filled resin layer can be taken out in one step of pulling up the porous plate. In addition, since there are few decomposed parts, contamination such as dust and bacteria can be minimized. In addition, by adjusting the number of perforated plates and consolidation plates according to the ring-layer type or multi-layer type of the circular ring chromatography device,
It can be applied to any type of circular chromatography device.

[0017]

According to the present invention, the perforated plate is lowered into the space between the outer cylinder and the inner cylinder, and the resin slurry is filled and compacted while being entrained with the perforated plate to uniformly fill the narrow space. Since the layer can be formed and the filled resin layer can be taken out in one step of raising the perforated plate, it is possible to form and take out the filled resin layer while suppressing contamination of dust and miscellaneous bacteria to a minimum.

[Brief description of drawings]

FIG. 1 is a sectional view showing an embodiment of the present invention.

2 is a cross-sectional view in which a filling resin layer of FIG. 1 is formed.

3 is a cross-sectional view showing the consolidation mechanism of FIG.

FIG. 4 is a cross-sectional view showing a conventional circular chromatography apparatus.

[Explanation of symbols]

 1 Void 2 Perforated Plate 3 Lifting Mechanism 4 Support Rod 6 Resin Slurry 7 Resin Injection Pipe 8 Center Rotation Shaft 9 Injection Pipe Support Arm 30 Consolidation Mechanism

Claims (2)

[Claims] 1. A perforated plate capable of ascending and descending a space between an outer cylinder and an inner cylinder, an elevating mechanism for supporting the perforated plate at its lower end to elevate and lower into the space, and the perforated plate as the perforated plate descends. A resin injection pipe for injecting the resin slurry into the upper part of the plate, an injection pipe support arm for connecting the resin injection pipe to the central rotating shaft to rotate it, and consolidating the resin slurry filled in the void through the porous plate. A resin filling device for a ring chromatography device, which comprises a compaction mechanism formed in a filled resin layer. 2. A porous plate is lowered into a space between an outer cylinder and an inner cylinder, and with the lowering, a resin slurry is injected into an upper portion of the porous plate through a resin injection pipe, and the resin injection pipe is Characterized in that the resin slurry is rotated together with a central rotating shaft to consolidate the resin slurry filled in the voids via the porous plate to form a filled resin layer, and the porous plate is raised to take out the filled resin layer. Resin filling method for circular ring chromatography.