阅读说明：本技术 管柱、管柱填充装置、管柱填充系统以及管柱处理方法 (Pipe column, pipe column filling device, pipe column filling system and pipe column processing method ) 是由 山中直树 户所正美 于 2019-06-06 设计创作，主要内容包括：本发明获得一种可将填充剂迅速且容易地填充至色谱法用管柱的管柱、管柱填充装置、管柱填充系统以及管柱处理方法。管柱填充装置主要包括：槽、作为搅拌机的搅拌器、泵、树脂瓶、第一配管～第十一配管、包含三通阀的第一阀～第四阀、以及包含二通阀的第五阀及第六阀。在第五配管的前端安装吸入口,吸入口从树脂瓶的顶部开口插入内部。第五配管的另一端与第一阀连接。第一阀与第一配管、第二配管、及第五配管连接,将这些配管相互连接或切断。第一配管的一端安装在槽的底部附近,并在槽的内侧底面附近开口。(the invention provides a column, a column filling device, a column filling system and a column processing method, wherein a filling agent can be quickly and easily filled into a column for chromatography. The tubular column filling device mainly comprises: a tank, a stirrer as a stirrer, a pump, a resin bottle, first to eleventh pipes, first to fourth valves including a three-way valve, and fifth and sixth valves including a two-way valve. A suction port is attached to the front end of the fifth pipe, and the suction port is inserted into the resin bottle from the top opening thereof. The other end of the fifth pipe is connected to the first valve. The first valve is connected to the first pipe, the second pipe, and the fifth pipe to connect and disconnect the pipes to each other. One end of the first pipe is attached near the bottom of the tank and opens near the inner bottom of the tank.)

1. A column packing apparatus, comprising:

A tank for storing the liquid and the filler;

A transfer pipe for transferring the slurry obtained by mixing the liquid and the filler from the tank to the column; and

A return conduit for returning the slurry from the column to the tank.

2. The tubular string filling apparatus according to claim 1,

The transfer line flows the slurry into the column from above a fill completion location of the packing in the column.

3. The string filling apparatus according to claim 1 or 2,

The return pipe takes out the slurry from the column from a position further above a filling completion position of the packing in the column.

4. The string filling apparatus according to claim 1 or 2,

The transfer pipe takes out the slurry from the vicinity of the bottom of the tank.

5. The string filling apparatus according to claim 1 or 2,

The transfer line includes a pump that transfers the slurry from the trough toward the tubing string.

6. The string filling apparatus according to claim 1 or 2,

The apparatus further comprises a stirrer disposed in the tank for mixing the liquid with the filler.

7. The string filling apparatus according to claim 1 or 2, characterized by further comprising:

a container holding the liquid and the filler;

a container removal tube for removing the liquid and the filler from the container; and

A container return pipe that returns the liquid and the filler, which have been taken out by the container take-out pipe, to the container;

the transfer pipe includes a pump that pressure-feeds the slurry from the tank toward the pipe string, a first valve provided between the tank and the pump, and a second valve provided between the pump and the pipe string,

the container removal tube is connected to the first valve,

the tank return line is connected to the second valve,

The first valve closing the path of the transport tube to the tank and opening the path of the transport tube to the container take-off tube,

The second valve closing the path of the transfer line to the tubing string and opening the path of the transfer line to the container return line,

The pump takes out the liquid and the filler from the container via the container take-out pipe, and returns the liquid and the filler to the container via the container return pipe.

8. The string filling apparatus according to claim 1 or 2, comprising:

A container holding the liquid and the filler; and

A container take-out pipe for taking out the liquid and the filler from the container;

the transfer pipe includes a pump that pumps the slurry from the tank toward the column, a first valve provided between the tank and the pump, and a third valve provided between the pump and the column,

The return pipe includes a fourth valve disposed between the pipe string and the tank, and

Includes a pipe connecting the third valve and the fourth valve,

The container removal tube is connected to the first valve,

The first valve closes a path of the transport pipe to the tank and opens a path of the container take-out pipe to the transport pipe,

The third valve closes a path of the transport pipe to the column and opens a path from the pump to the piping,

the fourth valve closes a path of the return pipe to the column and opens a path of the return pipe to the tank,

The pump takes out the liquid and the filler from the container through the container take-out pipe, and transfers the liquid and the filler to the tank.

9. The string filling apparatus according to claim 1 or 2, further comprising:

a container holding the liquid and the filler;

A tank take-out pipe for taking out the liquid from the tank; and

A tank return pipe that returns the liquid that has been taken out by the tank take-out pipe to the tank;

The transfer pipe includes a pump that pressure-feeds the slurry from the tank toward the pipe string, a first valve provided between the tank and the pump, and a second valve provided between the pump and the pipe string,

The tank withdrawal line is connected to the first valve,

The tank return line is connected to the second valve,

The first valve closing the path of the transport pipe to the tank and opening the path of the transport pipe to the tank take-off pipe,

The second valve closing the path of the transfer line to the tubing string and opening the path of the transfer line to the container return line,

The pump takes out the liquid from the tank through the tank take-out pipe and discharges the liquid to the outside through the tank return pipe, thereby adjusting the concentration of the filler with respect to the liquid.

10. the string filling apparatus according to claim 1 or 2,

The device also comprises a column bottom valve arranged at the bottom of the column, and the column bottom valve enables the liquid in the column to flow out towards the outside.

11. the string filling apparatus according to claim 1 or 2,

further comprising a tank withdrawal pipe for withdrawing said liquid from said tank,

The transfer pipe includes a pump that pressure-feeds the slurry from the tank toward the string, and a first valve provided between the tank and the pump,

The tank withdrawal line is connected to the first valve,

The first valve closing the path of the transport pipe to the tank and opening the path of the transport pipe to the tank take-off pipe,

the pump taking out the liquid from the tank through the tank take-out pipe and discharging the liquid toward the column through the transfer pipe to mix the packing agent in the column with the liquid to form a slurry,

the return line returns the slurry from the column to the tank.

12. the string filling apparatus according to claim 1 or 2,

Further comprising a tank withdrawal pipe for withdrawing said liquid from said tank,

the transfer pipe includes a pump for pumping the slurry from the tank to the pipe string, and a second valve provided between the pump and the pipe string, and

Further comprising a column bottom valve provided at the bottom of the column to allow the liquid in the column to flow out to the outside, and a column bottom connecting pipe connecting the second valve and the column bottom valve,

The second valve opens the path of the transfer line to the string bottom connection pipe,

The pump takes out the liquid from the tank through the tank take-out pipe, and injects the liquid from the bottom of the column toward the inside through the column bottom connection pipe and the column bottom valve.

13. The string filling apparatus according to claim 1 or 2, further comprising:

A container take-out tube for taking out at least the liquid from the column; and

A container return pipe that returns the liquid that has been taken out by the container take-out pipe to the column;

the transfer pipe includes a pump that pressure-feeds the slurry from the tank toward the pipe string, a first valve provided between the tank and the pump, and a second valve provided between the pump and the pipe string,

The container removal tube is connected to the first valve,

The tank return line is connected to the second valve,

The first valve closing the path of the transport tube to the tank and opening the path of the transport tube to the container take-off tube,

the second valve closing the path of the transfer line to the tubing string and opening the path of the transfer line to the container return line,

the pump extracts at least the liquid from the column via the vessel withdrawal line and returns the liquid to the column via the vessel return line, mixing the packing agent within the column with the liquid to form a slurry.

14. The string filling apparatus according to claim 1 or 2,

The slurry level in the tank is arranged above a liquid level in the column, which level discharges the liquid to the outside, in the direction of gravity.

15. A method of string treatment, comprising:

a step of storing the liquid and the filler in a tank;

Transferring a slurry obtained by mixing the liquid and the filler from the tank to a column; and

A step of returning the slurry from the column to the tank.

16. A pipe string, comprising:

A tubular column body capable of filling the filler to a filling completion position; and

and a pipe mounting port provided on a side surface of the pipe column body and provided between an axial end portion on a side close to the filling completion position and the filling completion position.

17. The pipe string of claim 16,

Comprises a piston which is movable in the axial direction within the column body and which is capable of compressing the filling agent, and

The piston is movable beyond the filling completion position from an axial end portion on the side close to the filling completion position.

18. a tubular column packing system, comprising:

A column including a tubular column body; and

The tubular string filling device of claim 1;

The column packing device comprises a cap which detachably blocks an axial end of the column body, and

the delivery pipe and the return pipe penetrate through the cover and are inserted into the pipe column body.

19. A tubular column packing system, comprising:

The pipe string filling apparatus of claim 1, and the pipe string of claim 16.

Technical Field

the present invention relates to a column used in a column for chromatography, a column packing device, a column packing system, and a column processing method.

background

Previously, a method of filling a packing material into a column used in chromatography has been known. The column is a tube having a filter at one end, and is provided so that the axial direction thereof is vertical and the end portion where the filter is provided is vertically upward. Then, the slurry is injected from the lower end in the direction of gravity toward the column. At this time, the filter does not allow the filler to permeate but only the liquid, so that the filler does not flow out from the upper end of the column but only the liquid flows out. Therefore, the packing remains in the column and precipitates (see patent document 1).

[ Prior art documents ]

[ patent document ]

Patent document 1: japanese patent laid-open publication No. 2002-531848

Disclosure of Invention

[ problems to be solved by the invention ]

However, as the packing agent precipitates in the column, the thickness of the packing agent increases, whereby it becomes difficult for liquid to permeate through the layer of the packing agent, the resistance to injection of the slurry into the column increases, and the injection rate of the slurry decreases. When the injection speed is decreased, the flow speed in the pipe connecting the tank storing the slurry and the column is also decreased, and therefore, the pipe may be clogged with the filler.

the present invention has been made in view of the above problems, and an object of the present invention is to provide a column, a column packing device, a column packing system, and a column processing method, which can quickly and easily pack a packing material into a chromatography column.

[ means for solving problems ]

The present invention includes the following [1] to [19 ].

[1] A column packing apparatus, comprising: a tank for storing the liquid and the filler; a transfer pipe for transferring the slurry obtained by mixing the liquid and the filler from the tank to the column; and a return conduit for returning the slurry from the column to the tank.

[2] The column packing apparatus according to [1], wherein the transfer pipe flows the slurry into the column from above a packing completion position of the packing agent in the column.

[3] the column packing device according to [1] or [2], wherein the return pipe takes out the slurry from the column from above a packing completion position of the packing agent in the column.

[4] The column packing apparatus according to any one of [1] to [3], wherein the transfer line takes out the slurry from near a bottom of the tank.

[5] the column filling apparatus according to any one of [1] to [4], wherein the transfer pipe includes a pump that transfers the slurry from the tank toward the column.

[6] The column packing apparatus according to any one of [1] to [5], further comprising a stirrer provided in the tank for mixing the liquid and the filler.

[7] The column packing apparatus according to any one of [1] to [6], further comprising: a container holding the liquid and the filler; a container take-out pipe for taking out the liquid and the filler from the container; and a container return pipe that returns the liquid and the filler, which have been taken out by the container take-out pipe, to the container; the transport pipe includes a pump for pumping the slurry from the tank to the column, a first valve provided between the tank and the pump, and a second valve provided between the pump and the column, the container take-out pipe is connected to the first valve, the container return pipe is connected to the second valve, the first valve closes a path between the transport pipe and the tank and opens a path between the transport pipe and the container take-out pipe, the second valve closes a path between the transport pipe and the column and opens a path between the transport pipe and the container return pipe, and the pump takes out the liquid and the filler from the container via the container take-out pipe and returns the liquid and the filler to the container via the container return pipe.

[8] The column packing apparatus according to any one of [1] to [7], comprising: a container holding the liquid and the filler; and a container take-out pipe that takes out the liquid and the filler from the container; the transfer pipe includes a pump that pumps the slurry from the tank to the column, a first valve provided between the tank and the pump, and a third valve provided between the pump and the column, the return pipe includes a fourth valve provided between the column and the tank, and includes a pipe that connects the third valve and the fourth valve, the container take-out pipe is connected to the first valve, the first valve closes a path of the transfer pipe to the tank and opens a path from the container take-out pipe to the transfer pipe, the third valve closes a path of the transfer pipe to the column and opens a path from the pump to the pipe, the fourth valve closes a path of the return pipe to the column and opens a path from the pipe to the tank, and the pump takes out the liquid and the filler from the container via the container take-out pipe, and transferred to the tank.

[9] the column packing apparatus according to any one of [1] to [8], further comprising: a container holding the liquid and the filler; a tank take-out pipe for taking out the liquid from the tank; and a container return pipe that returns the liquid that has been taken out by the tank take-out pipe to the container; the transport pipe includes a pump for pumping the slurry from the tank to the column, a first valve provided between the tank and the pump, and a second valve provided between the pump and the column, the tank take-out pipe is connected to the first valve, the tank return pipe is connected to the second valve, the first valve closes a path between the transport pipe and the tank and opens a path between the transport pipe and the tank take-out pipe, the second valve closes a path between the transport pipe and the column and opens a path between the transport pipe and the tank return pipe, and the pump takes out the liquid from the tank via the tank take-out pipe and discharges the liquid to the outside via the tank return pipe, thereby adjusting the concentration of the filler with respect to the liquid.

[10] The column packing apparatus according to any one of [1] to [9], further comprising a column bottom valve provided at a bottom of the column, the column bottom valve allowing the liquid in the column to flow out to the outside.

[11] The column packing apparatus according to any one of [1] to [10], further comprising a tank extraction pipe that extracts the liquid from the tank, wherein the transfer pipe includes a pump that pumps the slurry from the tank to the column and a first valve provided between the tank and the pump, wherein the tank extraction pipe is connected to the first valve, the first valve closes a path between the transfer pipe and the tank and opens a path between the transfer pipe and the tank extraction pipe, the pump extracts the liquid from the tank via the tank extraction pipe and discharges the liquid to the column via the transfer pipe, and the filler in the column and the liquid are mixed to form a slurry, and the return pipe returns the slurry from the column to the tank.

[12] The column packing apparatus according to any one of [1] to [10], further comprising a tank extraction pipe that extracts the liquid from the tank, wherein the transfer pipe includes a pump that pumps the slurry from the tank to the column, and a second valve provided between the pump and the column, and further comprises a column bottom valve provided at a bottom of the column and that allows the liquid in the column to flow out, and a column bottom connection pipe that connects the second valve to the column bottom valve, wherein the second valve opens a path between the transfer pipe and the column bottom connection pipe, and wherein the pump extracts the liquid from the tank via the tank extraction pipe and injects the liquid from the bottom of the column to an inside via the column bottom connection pipe and the column bottom valve.

[13] the column packing apparatus according to any one of [1] to [10], further comprising: a container take-out tube for taking out at least the liquid from the column; and a container return pipe that returns the liquid that has been taken out by the container take-out pipe to the column; the transfer pipe includes a pump that pressure-feeds the slurry from the tank toward the pipe string, a first valve provided between the tank and the pump, and a second valve provided between the pump and the pipe string, the container take-out pipe is connected to the first valve, the container return pipe is connected to the second valve, and the first valve closes a path between the transport pipe and the tank, and opening the path of the transfer line and the container withdrawal line, the second valve closing the path of the transfer line and the tubing string, and opening the path of the transfer pipe and the container return pipe, the pump taking out at least the liquid from the column via the container take-out pipe, and returning the liquid to the column via the vessel return line, the packing agent within the column being mixed with the liquid to form a slurry.

[14] The column packing device according to any one of [1] to [13], wherein a slurry level in the tank is disposed above a liquid level in the column, the liquid level discharging the liquid to the outside, in a gravity direction.

[15] A method of string treatment, comprising: a step of storing the liquid and the filler in a tank; transferring a slurry obtained by mixing the liquid and the filler from the tank to a column; and a step of returning the slurry from the column to the tank.

[16] A tubular string, comprising: a tubular column body capable of filling the filler to a filling completion position; and a pipe attachment port provided on a side surface of the column body and provided between an axial end portion on a side close to the completion position and the completion position.

[17] the column according to [16], which comprises a piston that is movable in an axial direction within the column body and that can compress the filling agent, and that is movable beyond the filling completion position from an axial end on a side close to the filling completion position.

[18] a tubular column packing system, comprising: a column including a tubular column body; and the column packing device described in [1 ]; the column packing device includes a cover that detachably blocks an axial end portion of the column body, and the transport pipe and the return pipe are inserted into the column body through the cover.

[19] A tubular column packing system, comprising: [1] the column packing device according to [1] and the column according to [16 ].

[ Effect of the invention ]

According to the present invention, a column packing device, a column packing system, and a column processing method are obtained, by which a packing material can be quickly and easily packed into a chromatography column.

drawings

Fig. 1 is a block diagram of a pipe column packing apparatus of a first embodiment.

Fig. 2 is a flowchart showing a pipe string processing method.

FIG. 3 is a block diagram of a column packing apparatus in a process of generating a slurry.

Fig. 4 is a block diagram of a column packing apparatus in a process of transferring slurry to a tank.

fig. 5 is a block diagram of a column packing apparatus in a process of adjusting the concentration of a slurry.

Fig. 6 is a block diagram of a column packing apparatus in a process of transferring a slurry to a first column.

FIG. 7 is a block diagram of a column packing apparatus in a process of precipitating a packing agent in a first column.

fig. 8 is a block diagram of a column packing apparatus in a process of recovering a packing agent from a first column.

fig. 9 is a block diagram of a column packing apparatus in a process of recovering a packing agent from a first column.

Fig. 10 is a block diagram of a column packing apparatus in a process of recovering a packing agent from a first column.

FIG. 11 is a block diagram of a second embodiment tubular string packing apparatus including a second tubular string.

FIG. 12 is a cross-sectional view of the second tubular string in a plane orthogonal to the axis of the second tubular string.

FIG. 13 is a cross-sectional view of the second string in a plane orthogonal to the axis of the second string.

Fig. 14 is a graph showing a temporal change in the amount of water discharged from the fifth valve.

Fig. 15 is a graph showing the results of chromatography after filling.

[ description of symbols ]

10: tubular column filling system

11: tubular column filling device

12: first tubular column

22: second tubular column

111: trough

112: stirrer

112 a: rotating shaft

112 b: stirring bar

113: pump and method of operating the same

114: resin bottle

115: vent port

116: discharge port

117: suction inlet

118: suction inlet with filter

121: first tubular column

122: cover

123: filter

221: second tubular column

221 a: filler filled region

222: cover

223: adapter

223 a: piston

223 b: inflow pipe

224: joint cartridge

Detailed Description

The first column 12, the column packing device 11, and the column packing system 10 according to the present invention will be described below with reference to fig. 1 to 3. The string filling system 10 basically includes a string filling device 11 and a first string 12.

The column packing device 11 mainly includes: the tank 111, a stirrer 112 as a stirrer, a pump 113, a resin bottle 114, first to eleventh pipes L1 to L11, first to fourth valves V1 to V4 including three-way valves, and fifth and sixth valves V5 and V6 including two-way valves. The fifth valve V5 forms a column bottom valve. The resin bottle 114 is a container for storing a slurry containing a filler and a liquid, and is shown as a container in fig. 2. The filler includes a resin, and includes, for example, cellulose, agarose, and a polymer (acrylic polymer or the like). A suction port 117 is attached to the tip of the fifth pipe L5, and the suction port 117 is inserted into the resin bottle 114 from the top opening thereof. The other end of the fifth pipe L5 is connected to the first valve V1. The first valve V1 is connected to the first pipe L1, the second pipe L2, and the fifth pipe L5, and connects and disconnects these pipes to and from each other. One end of the first pipe L1 is attached near the bottom of the tank 111 and opens near the inner bottom surface of the tank 111.

The tank 111 is a container having a predetermined capacity, and includes a vent 115 opened to the atmosphere. The stirrer 112 is inserted from the outside of the tank 111. The agitator 112 includes an agitator 112b attached to a front end of the rotating shaft 112a, and the agitator 112b is rotated by the rotating shaft 112a to agitate the slurry stored in the tank 111. The tenth pipe L10 is inserted from the top of the tank 111, and the tip of the tenth pipe L10 extends to the vicinity of the inner bottom surface of the tank 111.

The tenth pipe L10 is a three-way pipe, and has one end connected to the tank 111, one end connected to the sixth valve V6, and the remaining end connected to the fourth valve V4. The sixth valve V6 is provided above the first column 12 in the gravity direction, and is connected to the tenth pipe L10 and the eleventh pipe L11 to connect and disconnect the pipes to and from each other. One end of the eleventh pipe L11 is open to the atmosphere. The fourth valve V4 is connected to a tenth pipe L10, an eighth pipe L8, and a ninth pipe L9, and connects and disconnects these pipes to each other. The other end of the eighth pipe L8 is connected to the third valve V3, and the other end of the ninth pipe L9 is connected to the first column 12 described later. The third valve V3 is connected to the eighth pipe L8, the seventh pipe L7, and the sixth pipe L6, and connects and disconnects these pipes to each other. The other end of the sixth pipe L6 is connected to the second valve V2, and the other end of the seventh pipe L7 is connected to the first column 12 described later. The second valve V2 is connected to the third pipe L3, the fourth pipe L4, and the sixth pipe L6, and connects and disconnects these pipes to each other. The other end of the third pipe L3 is connected to the pump 113. A fifth valve V5 is connected to the bottom of the first column tube 121.

The pump 113 is a bidirectional pump, and is connected to the second pipe L2 and the third pipe L3, and pumps a liquid, slurry, or the like from the second pipe L2 to the third pipe L3, or pumps a liquid, slurry, or the like from the third pipe L3 to the second pipe L2. A discharge port 116 is provided at the other end of the fourth pipe L4, and the discharge port 116 is inserted into the resin bottle 114 from the top opening thereof.

The first pipe string 12 mainly includes: a first column tube 121 having a cylindrical shape with a bottom, a cover 122, and a filter 123. The filter 123 is a disc-shaped filter having a pore size to the extent that liquid can pass but the filler cannot pass. The outer diameter of the filter 123 is substantially the same as the inner diameter of the first column tube 121. The filter 123 is inserted from the top opening before the filler is transferred into the first column tube 121, and is closely attached to the inner bottom surface. Thus, liquid can pass through the first column tube 121 toward the fifth valve, and the filler cannot pass through the liquid. The cover 122 is connected to the seventh pipe L7 and the ninth pipe L9, is detachably attached to the top opening of the first column pipe 121, and closes one end of the first column pipe 121 in the axial direction. In this state, the tip of the seventh pipe L7 penetrates the cover 122, reaches the inside from the outside of the first column 12, and is provided in such a shape and position as to be swirled by the slurry discharged from the tip inside the first column pipe 121. The tip of the ninth pipe L9 is provided so as to penetrate the cover 122 to a position where the cover 122 is substantially flush with the surface inside the first column 12. The first column tube 121 forms a column body.

Next, a column processing method performed by the column packing device and the column packing system will be described with reference to fig. 2 to 10.

Fig. 2 is a flowchart showing a pipe string processing method. Steps S21 to S26 show a process of filling the first column 12 with the slurry, and steps S28 and S29 show a process of recovering the slurry from the first column 12. First, step S21 to step S26 will be described with reference to fig. 2 to 7.

The first step S21 is the following processing: the filler and the liquid in the resin bottle 114 are stirred to generate fluidity, thereby generating slurry. Step S21 is explained below with reference to fig. 3. In this process, the first valve V1 opens the path between the fifth pipe L5 and the second pipe L2 and closes the path between the fifth pipe L5 and the second pipe L2 and the first pipe L1. The second valve V2 opens the path between the third pipe L3 and the fourth pipe L4 and closes the path between the third pipe L3 and the fourth pipe L4 and the sixth pipe L6. Thus, the suction port 117 is connected to the discharge port 116 via the fifth pipe L5, the first valve V1, the second pipe L2, the pump 113, the third pipe L3, the second valve V2, and the fourth pipe L4. The piping, pump, and valve from suction port 117 to discharge port 116 are filled with the liquid constituting the slurry. In this state, when the pump 113 is operated so that the liquid flows from the second pipe L2 to the third pipe L3, the liquid in the resin bottle 114 is sucked from the suction port 117, passes through the pipe, the pump, and the valve, and is discharged from the discharge port 116 into the resin bottle 114. The filler in the resin bottle 114 is stirred with the liquid by the flow of the discharged liquid. When this operation is continued for a predetermined time, the filler is mixed with the liquid to produce a slurry. At this time, the fifth pipe L5 forms a container take-out pipe, and the fourth pipe L4 forms a container return pipe.

Step S22 is a process of transferring the slurry in the resin bottle 114 to the tank 111. Step S22 will be described below with reference to fig. 4. In this process, the first valve V1 opens the path between the fifth pipe L5 and the second pipe L2 and closes the path between the fifth pipe L5 and the second pipe L2 and the first pipe L1. The second valve V2 opens the path between the third pipe L3 and the sixth pipe L6 and closes the path between the third pipe L3 and the sixth pipe L6 and the fourth pipe L4. The third valve V3 opens the path of the sixth pipe L6 and the eighth pipe L8 and closes the path of the sixth pipe L6, the eighth pipe L8, and the seventh pipe L7. The fourth valve V4 opens the path of the eighth pipe L8 and the tenth pipe L10 and closes the path of the eighth pipe L8, the tenth pipe L10 and the ninth pipe L9. The sixth valve V6 is closed, and the path between the tenth pipe L10 and the eleventh pipe L11 is closed. Thus, the suction port 117 is connected to the tank 111 via the fifth pipe L5, the first valve V1, the second pipe L2, the pump 113, the third pipe L3, the second valve V2, the sixth pipe L6, the third valve V3, the eighth pipe L8, the fourth valve V4, and the tenth pipe L10. In this state, when the pump 113 is operated so that the liquid flows from the second pipe L2 to the third pipe L3, the slurry in the resin bottle 114 is sucked from the suction port 117, passes through the pipe, the pump, and the valve, and is discharged from the tenth pipe L10 into the tank 111. This operation is continued for a predetermined time, and the slurry in the resin bottle 114 is transferred to the tank 111.

Step S23 is a process of adjusting the concentration of the slurry in the tank 111. Step S23 is explained below with reference to fig. 5. First, the tank 111 is left to stand to completely precipitate the filler, and then the volume of the filler in the tank 111 is measured based on the volume of the precipitated filler. Scales, not shown, are provided in the groove 111, and the volume of the filler can be easily measured by referring to the scales.

then, the amount of the liquid in the tank is adjusted so that the concentration of the filler in the slurry becomes a desired concentration. The details will be described below. Here, the first valve V1 opens the path between the fifth pipe L5 and the second pipe L2 and closes the path between the fifth pipe L5 and the second pipe L2 and the first pipe L1. The second valve V2 opens the path between the third pipe L3 and the fourth pipe L4 and closes the path between the third pipe L3 and the fourth pipe L4 and the sixth pipe L6. Thus, the suction port 117 is connected to the discharge port 116 via the fifth pipe L5, the first valve V1, the second pipe L2, the pump 113, the third pipe L3, the second valve V2, and the fourth pipe L4. Then, suction port 117 is drawn out of resin bottle 114 and inserted into groove 111. At this time, the fifth pipe L5 forms a tank take-out pipe, and the fourth pipe L4 forms a tank return pipe. In this state, when the pump 113 is operated so that the liquid flows from the second pipe L2 to the third pipe L3, the liquid in the tank 111 is sucked from the suction port 117, passes through the pipes, the pump, and the valve, and is discharged from the discharge port 116 into the resin bottle 114. This reduces the amount of liquid in the tank 111. On the other hand, when the pump 113 is operated so that the liquid flows from the third pipe L3 to the second pipe L2, the liquid in the resin bottle 114 is sucked from the discharge port 116, passes through the pipes, the pump, and the valve, and is discharged from the suction port 117 into the tank 111. This increases the liquid in the tank 111. These operations are continued for a predetermined time, and the amount of the liquid in the tank 111 is adjusted so that the concentration of the filler in the slurry becomes a desired concentration. Here, the concentration is determined in consideration of the fluidity of the filler, and for example, a concentration of 50% by volume may be used. At 50% concentration, a slurry volume of twice the volume of the packing agent needs to be transferred into the first column 12. In addition, the amount of packing transferred into the first column 12 is less than the volume of the first column 12.

step S24 is a process of transferring the slurry in the tank 111 to the first column 12. Step S24 is explained below with reference to fig. 6. In this process, the first valve V1 opens the path of the first pipe L1 and the second pipe L2 and closes the path of the first pipe L1, the second pipe L2, and the fifth pipe L5. The second valve V2 opens the path between the third pipe L3 and the sixth pipe L6 and closes the path between the third pipe L3 and the sixth pipe L6 and the fourth pipe L4. The third valve V3 opens the path of the sixth pipe L6 and the seventh pipe L7, and closes the path of the sixth pipe L6, the seventh pipe L7, and the eighth pipe L8. The fourth valve V4 opens the path of the ninth pipe L9 and the tenth pipe L10 and closes the path of the ninth pipe L9, the tenth pipe L10 and the eighth pipe L8. The fifth valve V5 is closed. The sixth valve V6 is closed, and the path between the tenth pipe L10 and the eleventh pipe L11 is closed. Thus, the first pipe L1 attached near the bottom of the tank 111 is connected to the inside of the first column 12 via the first valve V1, the second pipe L2, the pump 113, the third pipe L3, the second valve V2, the sixth pipe L6, the third valve V3, and the seventh pipe L7, and the ninth pipe L9 connected to the first column 12 is connected to the inside of the tank 111 via the fourth valve V4 and the tenth pipe L10. Here, the first pipe L1, the second pipe L2, the third pipe L3, the sixth pipe L6, and the seventh pipe L7 form a transfer pipe, and the ninth pipe L9 and the tenth pipe L10 form a return pipe.

Then, first, the stirrer 112b is rotated to stir the slurry stored in the tank 111 for a predetermined time, thereby preparing a uniform slurry. Thereafter, when the pump 113 is operated so that the slurry flows from the second pipe L2 to the third pipe L3, the slurry in the tank 111 is sucked from the bottom of the tank 111 to the first pipe L1, passes through the pipes, the pump, and the valves, and is discharged from the seventh pipe L7 to the inside of the first column 12. Here, the seventh pipe L7 allows the slurry to flow in from above the filling completion position of the packing material in the first column 12. Thereby, the slurry in the tank 111 is transferred into the first column 12. Further, the air in the first column 12 flows into the tank 111 through the ninth pipe L9, the fourth valve V4, and the tenth pipe L10. As a result, the air pressure in the first column 12 rises and the air pressure in the tank 111 falls, so that the slurry in the tank 111 is smoothly transferred into the first column 12, and the first column 12 is filled with the slurry.

step S25 is a process of precipitating the packing agent in the first column 12. Step S25 is explained below with reference to fig. 7. This process differs from step S24 only in that the fifth valve V5 is opened, and the other pipes, pumps, and valves are connected in the same manner as in step S24. Here, for example, when 50% concentration slurry is transferred, when the first column 12 is filled with slurry, approximately the same amount of slurry as that in the first column 12 remains in the tank 111. Therefore, the stirrer 112b is rotated to stir the slurry in the tank 111, thereby preventing the filler from settling. At the same time, the pump 113 is operated in the same manner as in step S24 while the fifth valve V5 is opened, and the slurry in the tank 111 is transferred into the first column 12. The transferred slurry is returned to the tank 111 through the ninth pipe L9, the fourth valve V4, and the tenth pipe L10. Here, the ninth pipe L9 takes out the slurry from above the filling completion position of the packing agent in the first column 12. The liquid in the first column 12 is discharged to the outside through the filter 123 and the opened fifth valve V5, and the packing is stored in the first column 12. The filling completion position is a position where the filler is stored in the axial direction of the first column tube 121, and is a position determined in advance in anticipation of the filler being compressed in step S26 described later. Here, the slurry level in the tank 111, that is, the liquid upper surface of the slurry is arranged above the liquid surface discharged to the outside through the fifth valve V5 in the gravity direction. This applies a head pressure to the liquid in the first column 12, and the liquid in the first column 12 is quickly discharged to the outside.

As described above, in the conventional technique, as the packing agent precipitates in the column, the thickness of the packing agent becomes thick, and thus it becomes difficult for liquid to permeate through the layer of the packing agent, and the resistance to injection of the slurry into the column increases, and the injection rate of the slurry decreases, and the inside of the pipe may be clogged with the packing agent. However, according to the present embodiment, the slurry circulating through the tank 111 and the first column 12 does not permeate the precipitated packing agent, and the slurry flowing out from the first column 12 through the ninth pipe L9 is a supernatant of the slurry in the first column 12, and therefore, the concentration thereof is the concentration adjusted in the tank 111 in advance or less. Therefore, the flow velocity of the slurry in the pipe does not decrease, the slurry always flows, and the pipe is not clogged with the filler.

Step S26 is a process of packing the packing material by compressing the packing material optimally in the first string 12. In this process, the pipes, the pumps, and the valves are connected in the same manner as in step S25. After it was confirmed that substantially all of the packing in the tank 111 had settled in the first column 12, the fifth valve V5 was closed. Then, the cover 122 is detached from the first column tube 121, and an adaptor (adapter), not shown, is attached to the first column tube 121. The packing in the first string pipe 121 is compressed at a predetermined compression rate by attaching the adapter, thereby filling the packing into the first string 12. The compression ratio of the filler is determined in advance for each filler.

In step S27, the first column 12 is used for chromatography.

after the first column 12 is used for chromatography, the internal packing material is recovered and reused. Next, the process of collecting the packing from the first column 12 in steps S28 and S29 will be described with reference to fig. 8 to 10.

there are three different processes for the process of recovering the packing agent from the first column 12 of step S28. Hereinafter, various processes will be described.

First, the first recovery process will be described with reference to fig. 8. In the first recovery process, a suction port 118 with a filter is attached to the tip of the fifth pipe L5 instead of the suction port 117, and a cover 122 connected to the seventh pipe L7 and the ninth pipe L9 is attached to the top opening of the first column pipe 121. The first valve V1 opens the path between the fifth pipe L5 and the second pipe L2 and closes the path between the fifth pipe L5 and the second pipe L2 and the first pipe L1. The second valve V2 opens the path between the third pipe L3 and the sixth pipe L6 and closes the path between the third pipe L3 and the sixth pipe L6 and the fourth pipe L4. The third valve V3 opens the path of the sixth pipe L6 and the seventh pipe L7, and closes the path of the sixth pipe L6, the seventh pipe L7, and the eighth pipe L8. The fourth valve V4 opens the path of the ninth pipe L9 and the tenth pipe L10 and closes the path of the ninth pipe L9, the tenth pipe L10 and the eighth pipe L8. The fifth valve V5 is closed. The sixth valve V6 is closed, and the path between the tenth pipe L10 and the eleventh pipe L11 is closed. Thus, the suction port 118 with a filter is connected to the inside of the first column 12 via the fifth pipe L5, the first valve V1, the second pipe L2, the pump 113, the third pipe L3, the second valve V2, the sixth pipe L6, the third valve V3, and the seventh pipe L7, and the ninth pipe L9 connected to the first column 12 is connected to the inside of the tank 111 via the fourth valve V4 and the tenth pipe L10. At this time, the fifth pipe L5 forms a trough take-out pipe.

First, when the pump 113 is operated so that the liquid flows from the second pipe L2 to the third pipe L3, the liquid in the tank 111 is sucked into the fifth pipe L5 from the suction port 118 with a filter, passes through the pipes, the pump, and the valve, and is then discharged into the first column 12 from the seventh pipe L7. Thereby, the liquid in the tank 111 is transferred to the first column 12. The transferred liquid disturbs the filler filled in the first column 12 and fluidizes it. The fluidized filler is mixed with the liquid to become slurry, and flows into the tank 111 through the ninth pipe L9, the fourth valve V4, and the tenth pipe L10. Here, as described above, the tip of the seventh pipe L7 is provided in such a shape and position that the discharged liquid swirls in the first column pipe 121. Therefore, the liquid can efficiently disturb the filler to fluidize the filler.

When the first recovery process is started, the second valve V2 is set so as to open the path between the fourth pipe L4 and the third pipe L3 and close the path between the fourth pipe L4 and the third pipe L3 and the sixth pipe L6, and the pump 113 is operated so as to flow the slurry from the third pipe L3 to the second pipe L2. Thereby, the liquid in the resin bottle 114 is transferred into the tank 111 through the fourth pipe L4. In the first recovery process, the filler in the tank 111 is recovered using the liquid.

Next, the second recovery process will be described with reference to fig. 9. In the second recycling process, it is different from the first recycling process in the following respects: the second valve V2 opens a path between the third pipe L3 and the sixth pipe L6 and the fourth pipe L4, the fourth pipe L4 is connected to the fifth valve V5, and the fifth valve V5 opens a path between the fourth pipe L4 and the inside of the first column 12. Other pipes, pumps, and valves are connected in the same manner as in the first recovery process, and therefore, the description thereof is omitted. At this time, the fourth pipe L4 forms a column bottom connection pipe, and the fifth pipe L5 forms a trough extraction pipe.

First, when the pump 113 is operated so that the liquid flows from the second pipe L2 to the third pipe L3, the liquid in the tank 111 is sucked into the fifth pipe L5 from the suction port 118 with a filter, passes through the pipes, the pump, and the valve, and is then discharged into the first column 12 from the bottom of the seventh pipe L7 and the first column pipe 121. Thereby, the liquid in the tank 111 is transferred into the first column 12. The transferred liquid disturbs the filler filled in the first column 12 and fluidizes it. The fluidized filler is mixed with the liquid to become slurry, and flows into the tank 111 through the ninth pipe L9, the fourth valve V4, and the tenth pipe L10. Here, the liquid that has flowed in from the bottom of the first column tube 121 can be fluidized by disturbing the filler from the bottom, and the liquid that has been discharged from the tip of the seventh pipe L7 can be fluidized by disturbing the filler by flowing so as to swirl in the first column tube 121. By injecting the liquid from two directions, the filler can be efficiently mixed and fluidized for recovery.

Next, the third recovery process will be described with reference to fig. 10. In this process, the first valve V1 opens the path between the fifth pipe L5 and the second pipe L2 and closes the path between the fifth pipe L5 and the second pipe L2 and the first pipe L1. The second valve V2 opens the path between the third pipe L3 and the fourth pipe L4 and closes the path between the third pipe L3 and the fourth pipe L4 and the sixth pipe L6. At this time, the fourth pipe L4 forms a container return pipe, and the fifth pipe L5 forms a container take-out pipe.

thus, the suction port 117 is connected to the discharge port 116 via the fifth pipe L5, the first valve V1, the second pipe L2, the pump 113, the third pipe L3, the second valve V2, and the fourth pipe L4. The piping, pump, and valve from suction port 117 to discharge port 116 are filled with the liquid constituting the slurry. In this state, when the pump 113 is operated so that the liquid flows from the second pipe L2 to the third pipe L3, the liquid in the first column tube 121 is sucked from the suction port 117, passes through the pipes, the pump, and the valve, and is discharged from the discharge port 116 into the first column tube 121. The filler in the first column tube 121 is stirred with the liquid by the flow of the discharged liquid. When this operation is continued for a predetermined time, the filler is mixed with the liquid to produce a slurry. Then, the slurry is transferred into the tank 111 and recovered in the same manner as in step S22.

in step S29, the filler collected in the tank 111 is discarded or collected into the resin bottle 114 and stored. When the resin is recovered into the resin bottle 114, the first valve V1 opens the path between the first pipe L1 and the second pipe L2 and closes the path between the first pipe L1 and the second pipe L2 and the fifth pipe L5. The second valve V2 opens the path between the third pipe L3 and the fourth pipe L4 and closes the path between the third pipe L3 and the fourth pipe L4 and the sixth pipe L6. In this state, when the pump 113 is operated so that the liquid flows from the second pipe L2 to the third pipe L3 while the stirrer 112b is rotated to stir the slurry stored in the tank 111, the slurry in the tank 111 is sucked from the first pipe L1, passes through the pipes, the pump, and the valve, and is discharged from the discharge port 116 into the resin bottle 114 to be recovered.

According to the present embodiment, the filler does not stick to the inside of each pipe, the flow rate of the slurry inside the pipe decreases, or the pipe is clogged with the slurry, and the slurry can be stably transferred to the first column 12.

In step S23 of the column processing method, the volume of the packing material may be measured using a measuring instrument or the like provided in the tank 111 instead of the scale. In addition, in step S24, the fifth valve V5 may be opened. Thus, the liquid in the first column 12 permeates the filter 123 and is discharged to the outside, and only the packing agent is stored in the first column 12.

In the first to third recovery processes, the slurry in the tank 111 may be stirred by rotating the stirrer 112b as appropriate.

Next, a second column 22 according to a second embodiment will be described with reference to fig. 11 and 12. The second tubular string 22 mainly includes: a second column pipe 221 having a cylindrical shape with a bottom, a cover 222, a joint cylinder 224, and a filter 123. Fig. 12 is a cross-sectional view of a portion where the seventh pipe L7 and the ninth pipe L9 are connected to the second column pipe 221, cut along a plane perpendicular to the axis of the second column pipe 221.

The joint cylinder 224 is a cylindrical member having the same outer and inner diameters as the second string 22, and has two pipe attachment ports as through-holes on its side surface. The seventh pipe L7 and the ninth pipe L9 are connected to the respective pipe attachment ports via a two-way valve V3-1 and a two-way valve V4-1. An engagement cartridge 224 is mounted on top of the second tubing string 22 in such a way as to become coaxial with one another. In this state, the tip of the seventh pipe L7 penetrates the side surface, reaches the inner circumferential surface from the outside of the second column 22, does not protrude inward, and is provided in such a shape and position as to cause the slurry discharged from the tip to swirl in the second column pipe 221 (see fig. 12). In this state, the tube attachment opening is provided between the axial end portion of the second column tube 221 on the side close to the filling completion position and the filling completion position. In addition, in the present embodiment, the second column pipe 221 and the engagement cylinder 224 form a column body.

the cover 222 is made of resin or metal in a disk shape, and includes a hole penetrating along the central axis, and is installed at the top opening of the second column pipe 221. The adapter 223 includes a piston 223a and an inflow tube 223 b. Piston 223a is made of a disc-shaped resin or metal having a size that can be engaged with the inner peripheral surface of second column pipe 221, and includes a hole that penetrates in the axial direction along the central axis. The inflow pipe 223b is made of cylindrical resin or metal, and is connected to the piston 223a such that the hole of the piston 223a is connected to the inner circumference of the inflow pipe 223 b. The inflow pipe 223b is slidably inserted into a through hole provided in the cover 222. In a state where the cap 222 has been mounted on the second column pipe 221, the inflow pipe 223b is moved in the axial direction, whereby the piston 223a can be moved in the axial direction within the second column pipe 221. As described above, since the tip end of the seventh pipe L7 does not protrude into the second column 22, the piston 223a can move from the axial end portion of the second column pipe 221 on the side closer to the completion position to a position beyond the completion position.

When the piston 223a has been moved to the vicinity of the cap 222, the seventh pipe L7 and the ninth pipe L9 are connected to the filler filling region 221a in the second column pipe 221. In this state, the slurry can be filled or recovered into the second column pipe 221 through the seventh pipe L7 and the ninth pipe L9. On the other hand, when piston 223a has been moved into filler filling area 221a, piston 223a compresses the filler, thereby filling the filler into second column 22. At this time, the seventh pipe L7 and the ninth pipe L9 are cut from the filler filling region 221 a.

In steps S21 to S25, S27, and S29 in the column processing method, the second column 22 can be used in the same manner as in the first embodiment by moving the piston 223a to the vicinity of the cap 222. The description of these steps is omitted. In step S26 of the column processing method, the packing material is filled into the second column 22 by moving the piston 223a into the packing material filling region 221a without removing the cap 222, thereby compressing the packing material to a predetermined compression ratio by the piston 223 a.

Fig. 13 shows an example of a connection state of the seventh pipe L7 and the ninth pipe L9 to the second column 22, which is different from the connection state shown in fig. 12. Fig. 13 is a cross-sectional view of a portion where the seventh pipe L7 and the ninth pipe L9 are connected to the second column pipe 221, cut along a plane perpendicular to the axis of the second column pipe 221. In fig. 13, the seventh pipe L7 and the ninth pipe L9 are connected to the second stem 22 at an angle such that they are perpendicular to the axis of the second stem 22. The distal ends of the seventh pipe L7 and the ninth pipe L9 penetrate the side surface of the second stem 22 to reach the inner periphery, and do not protrude into the second stem 22. The outflow direction adjustment pipe 225 is attached to the inner periphery of the seventh pipe L7. The outflow direction adjustment pipe 225 has a tip end projecting toward the inside of the second string 22, and is covered so as to intercept the opening direction and open to the side. Thereby, the slurry discharged from the leading end swirls in the second column pipe 221.

According to the present embodiment, the same effects as those of the first embodiment are obtained. In addition, the packing agent may be filled into the second tubing string 22 without removing the cap 222.

in fig. 12 and 13, the tip of the seventh pipe L7 connected to the second column 22 and the tip of the ninth pipe L9 may be at the same position in the axial direction or may be provided at different positions. In fig. 12 and 13, the seventh pipe L7 and the ninth pipe L9 may be exchanged with each other. In fig. 13, the outflow direction adjustment pipe 225 may not be attached.

in any embodiment, a two-way valve may be used instead of a three-way valve. In this case, one two-way valve may be provided in each pipe.

the first column tube 121 and the second column tube 221 may not be made of resin, and may be made of a metal material or a glass material entirely or partially.

the outer diameter of the filter 123 may not be substantially the same as the inner diameter of the first column tube 121 and the second column tube 221. In this case, the outer diameter of the filter 123 may be as long as it is at least as long as the fifth valve V5 blocks the holes formed in the first column tube 121 and the second column tube 221, and the closer to the inner diameter of the first column tube 121 and the second column tube 221, the better. The outer diameter of the filter 123 may be embedded in a member forming the bottom of the first column tube 121 and the second column tube 221 with respect to the axial direction.

The stirrer 112 may be a magnetic stirrer (magnetic stirrer) instead of the stirrer including the stirrer 112b attached to the tip of the rotating shaft 112 a. In this case, a magnetic stirrer is disposed in the tank 111, and the slurry is stirred by rotating the stirrer through the wall of the tank 111 by magnetic force.

The tip of the seventh pipe L7 may have a linear shape instead of the shape and position of the swirl. The tip end of the seventh pipe L7 may not protrude into the first column 12, but may be provided so as to penetrate the lid 122 to a position where the lid 122 is substantially flush with the surface inside the first column 12.

In step S25, the sixth valve V6 may be opened or closed. As described above, the sixth valve V6 is disposed further upward in the gravitational direction than the first string 12. Therefore, when the sixth valve V6 is opened, atmospheric pressure is applied to the inside of the first column 12 through the tenth pipe L10 and the ninth pipe L9, thereby promoting the release of the liquid from the fifth valve V5. Thus, by opening or blocking the sixth valve V6, the rate of flow back of slurry from the first column 12 into the tank 111 can be adjusted. At this time, the sixth valve V6 is opened or closed so that the slurry is not discharged from the eleventh pipe L11. Alternatively, when the inner diameter of the pipe extending from the sixth valve V6 into the tank 111 is set to a value that does not impair the backflow of the slurry, the sixth valve V6 may be opened or omitted at all times, presumably because the slurry is not discharged from the eleventh pipe L11.