JPH0476627B2 - - Google Patents

Description

[Detailed Description of the Invention] <Industrial Application Field> This invention constructs a packed bed in a column of a chromatography device that separates target components from a stock solution containing multiple components by chromatography on an industrial scale. This invention relates to a method for removing filler.

<Prior art> The present applicant developed a chromatography device for separating target components from stock solutions on an industrial scale in 1980.
−162082, Patent Application No. 1984-84063, Patent Application No. 139269,
It was proposed in No. 145991.

<Problems to be Solved by the Invention> The packing material packed in the column has a usage limit, and its performance deteriorates after a certain period of use, so it is necessary to remove the packing material from the column and use new or recycled packing material. need to be refilled.

In this case, for analytical or small preparative columns with a diameter of 100 mm or less, the amount of solvent used is the smallest of the packing materials, so remove the lid from one end (lower end).
Water or solvent is pumped into the column from the stock solution inlet on the other end (upper end) of the lid, and the packing material is pushed out by the pressure of the pump into the receiving tank placed under the one end with the lid removed, which is relatively easy. can be taken out.

However, in large columns with a diameter of 100 mm or more, the amount of both packing material and solvent is large, so if you take it out as described above, the packing material will scatter and not enter the receiving tank, and the solvent will be removed. Gas also worsens the working environment.

To do this, remove the lid at the top of the column, tilt the column so that the opening at the top of the column faces sideways or downwards,
The packing material is washed out by spraying water onto the packed bed inside the column, or scraped out using a tool such as a ladle, but the hard and compacted packing material is difficult to remove, making the process difficult. In addition, the work environment is similarly deteriorated due to scattering of filler and generation of solvent gas.

<Means for solving the problem> Therefore, the method for removing the packing material from the chromatography apparatus of the present invention involves connecting a compressed air means to one end of the column, and supplying compressed air into the column from the compressed air supply means. The solvent in the column is forced out through the porous plate at the other end of the column, and then the porous plate is removed from the other end of the column, and compressed air is supplied from one end of the column to fill the column. It is characterized by extruding the agent.

<Example> In the illustrated example, 1 is a column containing a packed layer of filler, 2 and 3 are upper and lower lids of the column, and each lid is equipped with a dispersion plate 4 and a sintered material as is well known. A porous plate 5 made of metal is incorporated, and a dispersion plate 4
One end of the socket 6 communicating with the space is attached by screwing or the like and fixed to the column by flange connection.

A supply pipe 9 is connected to the other end of the socket 6 of the upper lid 2 via a three-way switching valve 7, which can switch between supplying the undiluted solution and compressed air from the compressor 8.
An extraction pipe 10 is connected to the other end of the socket 6 of the lower cover 3.

The connection of the piping 9 or 10 to the other end of each socket 6 may be by flange connection or screwing, but in this embodiment, an O-ring or packing 11 is inserted immediately after the part of the piping 9 or 10 that enters the socket. Fit,
This packing is screwed onto the tapered part of the inner periphery of the other end of the socket, and the cap nut 1 is screwed onto the outer periphery of the other end of the socket.
2 and presses the pipes 9 and 10 from around them with a gasket to seal and connect at the same time.

Incidentally, the column 1 is rotatably connected to the left and right stands 14 by the horizontal shaft 13, as in the above-mentioned Japanese Patent Application No. 139269/1983, and is configured to be able to reciprocate 180 degrees by the operation of the piston cylinder 15. .

To carry out the fractionation process, the three-way switching valve 7 supplies the stock solution into the column 1 through the supply pipe 9 and the upper lid 2, and the recovered liquid is discharged from the porous plate 5 of the lower lid 3 through the extraction pipe 10.

When the performance of the packing material deteriorates, the separation process is interrupted and the packing material inside the column is taken out. To do this, the three-way switching valve 7 is switched, the compressed air generated by operating the compressor 8 is supplied into the column through the supply pipe 9 and the upper lid 2, and the solvent in the column is transferred to the porous plate of the lower lid 3 by the compressed air. 5 to the extraction pipe 10. In this case, a three-way switching valve is also connected to the extraction pipe 10 as shown in the figure, and by switching the valve when interrupting the fractionation process, the extruded solvent can be recovered separately from the recovery liquid.

After almost all of the solvent in the column has been extruded in this way, pipes 9 and 10 are
, rotate the column 1 by 180 degrees with the piston cylinder 15 to turn it upside down, connect the pipe 9 to the socket of the lower cover facing upward, remove the upper cover 2 facing downward, and place the receiving tank 16 below it. (see Figure 3),
Compressed air is again blown into the column 1, and the compressed air forces the filler in the column into the receiving tank 16 below. After extrusion, the column is rotated 180 degrees again to stand upright, for example, in the above-mentioned patent application No.
As described in No. 145991, fill with a new or recycled filler using a colori pump or the like, attach the top cover 2, connect the pipes 9 and 10 as before, and restart the preparative separation process.

In this example, the column 1 was placed on the stand 14 so that it could be easily turned over, so it was rotated 180 degrees and turned upside down, and compressed air was blown into the column from the bottom cover. However, this is not necessary; While the column is held upright, compressed air may be blown into the column through the upper lid to extrude the solvent through the porous plate of the lower lid, and then the lower lid may be removed and compressed air may be blown through the upper lid again to extrude the filler. .

Furthermore, it is not always necessary to switch between the stock solution and compressed air using the three-way switching valve 7 to supply the column to the column; when interrupting the preparative separation process, the stock solution supply pipe can be removed from the socket on the top lid and the compressed air from the compressor can be switched off. The leading conduit may be reconnected to a socket on the top lid. Of course, when inverting the column after expelling the solvent from the column with compressed air, the compressed air conduit is removed from the socket in the upper lid and reconnected to the socket in the lower lid that faces upward after inversion.

<Effects of the Invention> According to the present invention, the solvent in the column is extruded in advance with compressed air, and then the lids at either end of the column are removed and compressed air is blown into the column again. Push the packing material out of the column.

Therefore, the scattering caused by taking out the solvent and the filler at the same time and the deterioration of the working environment due to the solvent gas do not occur, and the filler from the compacted packed bed can be easily taken out without requiring human power.

[Brief explanation of the drawing]

FIG. 1 is an overall view showing one embodiment of the present invention;
Fig. 2 is an enlarged cross-sectional view of a part of Fig. 1, and Fig. 3 is an explanatory view of the device in Fig. 1 taking out the packing material. In the figure, 1 is a column, 2 and 3 are The column has an upper cover and a lower cover, and numeral 8 indicates an air compressor for supplying compressed air.

Claims (1)

[Claims] 1 Connect a compressed air supply means to one end of the column, supply compressed air from the compressed air supply means into the column to extrude the solvent in the column through the porous plate at the other end of the column, and then A method for removing a filler in chromatography, which comprises removing a porous plate from the other end of the column and supplying compressed air into the column from one end to push out the filler in the column.