Patent Application
20190374875
This application claims the priority benefit of Japan application serial no. 2018-110250, filed on Jun. 8, 2018. The entirety of the above-mentioned patent application is hereby incorporated by reference herein and made a part of this specification.
The present invention relates to a column, a column filling apparatus, a column filling system, and a column processing method used for chromatography column.
Conventionally, a method for filling a filler in a column used for chromatography is known. The column has a cylindrical shape having an end provided with a filter, and is installed such that the axial direction thereof is along the vertical direction, and the end provided with the filter is located on a vertical upper side. Slurry is injected into the column from a lower end in the gravity direction. At this time, the filter does not transmit a filler, but transmits only liquid, and therefore the filler does not flow out from a column upper end, and only the liquid flows out. Therefore, the filler remains and settles in the column (refer to Japanese Publication of International Patent Application No. 2002-531848).
[PTL 1] Japanese Publication of International Patent Application No. 2002-531848).
However, as the filler settles in the column, the thickness of the filler increases. Consequently, the liquid is unlikely to be transmitted through layers of the filler, and resistance against injection of the slurry into the column increases, and the injection speed of the slurry reduces. When the injection speed reduces, the flow speed in a pipe connecting a container storing the slurry and the column becomes slow, and therefore a risk that the inside of the pipe is blocked by the filler occurs.
The present invention has been made in view of problems such as described above, and the present invention provides a column, a column filling apparatus, a column filling system, and a column processing method, in which a filler can be rapidly and easily filled in a chromatography column.
The invention of this application includes the following [1] to [19].
[1] A column filling apparatus comprising: a tank storing liquid and a filler; a transfer pipe transferring slurry from the tank to a column, the slurry comprising the liquid and the filler; and a reflux pipe for refluxing the slurry from the column to the tank.
[2] The column filling apparatus according to [1], wherein the transfer pipe allows the slurry to flow into the column from an upper side with respect to a filling completion position of a filler in the column.
[3] The column filling apparatus according to [1] or [2], wherein the reflux pipe takes out the slurry from the column from an upper side with respect to a filling completion position of a filler in the column.
[4] The column filling apparatus according to any one of [1] to [3], wherein the transfer pipe takes out the slurry from a vicinity of 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 to the column.
[6] The column filling apparatus according to any one of [1] to [5], further comprising an agitator that is provided in the tank, and mixes the liquid and the filler.
[7] The column filling apparatus according to any one of [1] to [6], further comprising: a container storing the liquid and the filler; a container take-out pipe taking out the liquid and the filler from the container; and a container return pipe returning, to the container, the liquid and the filler taken out by the container take-out pipe, wherein the transfer pipe includes a pump that pressure-feeds 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 transfer pipe and the tank, and opens a path between the transfer pipe and the container take-out pipe, the second valve closes a path between the transfer pipe and the column, and opens a path between the transfer pipe and the container return pipe, and the pump takes out the liquid and the filler from the container through the container take-out pipe, and returns the liquid and the filler to the container through the container return pipe.
[8] The column filling apparatus according to any one of [1] to [7], further comprising: a container storing the liquid and the filler; and a container take-out pipe taking out the liquid and the filler from the container, wherein the transfer pipe includes a pump that pressure-feeds 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 reflux pipe includes a fourth valve provided between the column and the tank, a pipe connecting the third valve and the fourth valve is provided, the container take-out pipe is connected to the first valve, the first valve closes a path to the tank in the transfer pipe, and opens a path from the container take-out pipe to the transfer pipe, the third valve closes a path to the column in the transfer pipe, and opens a path from the pump to the pipe, the fourth valve closes a path to the column in the reflux pipe, and opens a path from the pipe to the tank, and 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 column filling apparatus according to any one of [1] to [8], further comprising: a container storing the liquid and the filler; a tank take-out pipe taking out the liquid from the tank; and a container return pipe returning, to the container, the liquid taken out by the tank take-out pipe, wherein the transfer pipe includes a pump that pressure-feeds 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 container return pipe is connected to the second 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 take-out pipe, the second valve closes a path between the transfer pipe and the column, and opens a path between the transfer pipe and the container return pipe, and the pump takes out the liquid from the tank through the tank take-out pipe, discharges the liquid to outside through the container return pipe, and adjusts concentration of the filler to the liquid.
[10] The column filling apparatus according to any one of [1] to [9], further comprising a column bottom valve provided in a bottom of the column, wherein the column bottom valve allows the liquid in the column to flow out to outside.
[11] The column filling apparatus according to any one of [1] to [10], further comprising a tank take-out pipe that takes out the liquid from the tank, wherein the transfer pipe includes a pump that pressure-feeds the slurry from the tank to the column, and a first valve provided between the tank and the pump, the tank take-out 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 take-out pipe, the pump takes out the liquid from the tank through the tank take-out pipe, and discharges the liquid to the column through the transfer pipe, and produces slurry by mixing the filler and the liquid in the column, and the reflux pipe refluxes the slurry from the column to the tank.
[12] The column filling apparatus according to any one of [1] to [10], further comprising a tank take-out pipe that takes out the liquid from the tank, wherein the transfer pipe includes a pump that pressure-feeds the slurry from the tank to the column, and a second valve provided between the pump and the column, a column bottom valve that is provided in a bottom of the column, and allows the liquid in the column to flow out to outside, and a column bottom connection pipe connecting the second valve and the column bottom valve are further provided, the second valve opens a path between the transfer pipe and the column bottom connection pipe, and 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 to inside through the column bottom connection pipe and the column bottom valve.
[13] The column filling apparatus according to any one of [1] to [10], further comprising: a container take-out pipe that takes out at least the liquid from the column; and a container return pipe that returns, to the column, the liquid taken out by the container take-out pipe, wherein the transfer pipe includes a pump that pressure-feeds 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 transfer pipe and the tank, and opens a path between the transfer pipe and the container take-out pipe, the second valve closes a path between the transfer pipe and the column, and opens a path between the transfer pipe and the container return pipe, and the pump takes out at least the liquid from the column through the container take-out pipe, returns at least the liquid to the column through the container return pipe, and produces slurry by mixing the filler and the liquid in the column.
[14] The column filling apparatus according to any one of [1] to [13], wherein a slurry surface in the tank is disposed on an upper side in a gravity direction with respect to a liquid level at which the liquid is discharged to outside in the column.
[15] A column processing method comprising the steps of: storing liquid and a filler in a tank; transferring slurry from the tank to a column, the slurry comprising the liquid and the filler; and refluxing the slurry from the column to the tank.
[16] A column comprising: a cylindrical column body capable of filling a filler up to a filling completion position; and a pipe mounting port provided between an axial end near the filling completion position and the filling completion position on a side surface of the column body.
[17] The column according to [16], comprising a piston capable of axially moving inside the column body, and capable of compressing the filler, wherein the piston is capable of moving beyond the filling completion position from the axial end near the filling completion position.
[18] A column filling system comprising: a column comprising a cylindrical column body; and a column filling apparatus according to [1], wherein the column filling apparatus includes a lid that detachably blocks an axial end of the column body, and the transfer pipe and the reflux pipe penetrate the lid to be inserted into the column body.
[19] A column filling system comprising: a column filling apparatus according to [1]; and a column according to [16].
According to the present invention, a column, a column filling apparatus, a column filling system, and a column processing method, in which a filler can be rapidly and easily filled in a chromatography column, are obtained.
Hereinafter, a first column 12, a column filling apparatus 11, and a column filling system 10 according to the present invention will be described with reference to
The column filling apparatus 11 mainly includes a tank 111, a stirrer 112 being an agitator, a pump 113, a resin bottle 114, first to eleventh pipes L1 to L11, first to fourth valves V1 to V4 composed of three-way valves, and fifth and sixth valves V5, V6 composed of two-way valves. The fifth valve V5 forms a column bottom valve. The resin bottle 114 is a container storing slurry composed of filler and liquid, and is illustrated as a container in
The tank 111 is a container having predetermined capacity, and includes a vent port 115 opened to the atmosphere. The stirrer 112 is provided by being inserted from the outside of the tank 111. The stirrer 112 includes a stirring bar 112b mounted on a leading end of a rotary shaft 112a, and the stirring bar 112b is rotated by the rotary shaft 112a, and stirs slurry stored in the tank 111. A leading end of the tenth pipe L10 inserted from a top of the tank 111 extends up to the vicinity of the inner bottom surface of the tank 111.
The tenth pipe L10 is a three-way pipe, and has an end connected to the inside of the tank 111, an end connected to the sixth valve V6, and a remaining end connected to the fourth valve V4. The sixth valve V6 is installed on an upper side in the gravity direction with respect to the first column 12, is connected to the tenth pipe L10 and the eleventh pipe L11, and connects or disconnects these pipes to or from each other. An end of the eleventh pipe L11 is opened to the atmosphere. The fourth valve V4 is connected to the tenth pipe L10, the eighth pipe L8, and the ninth pipe L9, and connects or disconnects these pipes to or from 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 below. The third valve V3 is connected to the eighth pipe L8, the seventh pipe L7, and the sixth pipe L6, and connects or disconnects these pipes to or from 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 below. The second valve V2 is connected to the third pipe L3, the fourth pipe L4, and the sixth pipe L6, and connects or disconnects these pipes to or from each other. The other end of the third pipe L3 is connected to the pump 113. The fifth valve V5 is connected to a bottom of a first column tube 121.
The pump 113 is a bidirectional pump, is connected to the second pipe L2 and the third pipe L3, and pressure-feeds liquid, slurry or the like from the second pipe L2 to the third pipe L3, or from the third pipe L3 to the second pipe L2. A discharge port 116 is mounted on the other end of the fourth pipe L4, and the discharge port 116 is inserted into an inner part from the top opening of the resin bottle 114.
The first column 12 mainly includes the bottomed cylindrical first column tube 121, a lid 122, and a filter 123. The filter 123 is a disk-shaped filter having such a pore diameter as to enable passing of liquid but not as to enable passing of a filler. 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 provided so as to be in close contact with the inner bottom surface by being inserted from the top opening before the filler is transferred to the inside of the first column tube 121. Consequently, while the liquid can pass from the inside of the first column tube 121 toward the fifth valve, the filler cannot pass. The lid 122 is connected to the seventh pipe L7 and the ninth pipe L9, is detachably mounted on a top opening of the first column tube 121, and blocks an axial end of the first column tube 121. In this state, a leading end of the seventh pipe L7 penetrates the lid 122 to reach an inner part from an outer part of the first column 12, and is provided in such a shape and such a position that the slurry discharged from the leading end swirls inside the first column tube 121. A leading end of the ninth pipe L9 is provided so as to penetrate the lid 122 up to such a position as to be substantially flush with a surface inside the first column 12 in the lid 122. The first column tube 121 forms a column body.
Now, a column processing method implemented by a column filling apparatus and a column filling system will be described with reference to
Initial Step S21 is a process of stirring a filler and liquid in the resin bottle 114 to generate fluidity, and producing slurry. Hereinafter, Step S21 will be described with reference to
Step S22 is a process of transferring the slurry in the resin bottle 114 to the tank 111. Hereinafter, Step S22 will be described with reference to
Consequently, the suction port 117 is connected to the tank 111 through 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 driven such 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, and is discharged into the tank 111 from the tenth pipe L10 through the pipes, the pump, and the valves. This process is continued for a predetermined time, so that 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. Hereinafter, Step S23 will be described with reference to
Now, an amount of the liquid in the tank is adjusted, so that the concentration of the filler in the slurry is made to be desired concentration. Hereinafter, details will be described. Herein, 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. Additionally, 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. Consequently, the suction port 117 is connected to the discharge port 116 through 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 suction port 117 is pulled out from the resin bottle 114, and inserted into the tank 111. At this time, the fifth pipe L5 forms a tank take-out pipe, and the fourth pipe L4 forms a container return pipe. In this state, when the pump 113 is driven such that the liquid flows from the second pipe L2 to the third pipe L3, liquid in the tank 111 is sucked from the suction port 117, and is discharged into the resin bottle 114 from the discharge port 116 through the pipes, the pump, and the valves. Consequently, it is possible to reduce the amount of the liquid in the tank 111. On the other hand, when the pump 113 is driven such 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, and is discharged into the tank 111 from the suction port 117 through the pipes, the pump, and the valves. Consequently, it is possible to increase the amount of the liquid in the tank 111. These processes are continued for a predetermined time, so that the amount of the liquid in the tank 111 is adjusted, and the concentration of the filler in the slurry is made to be the desired concentration. Herein, the concentration is determined in consideration of the fluidity of the filler or the like, and for example, the concentration of 50 vol. % is used. In a case of the concentration of 50%, slurry whose volume is twice the filler to be transferred to the first column 12 is required. An amount of the filler to be transfer to 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. Hereinafter, Step S24 will be described with reference to
First, the stirring bar 112b is rotated, the slurry stored in the tank 111 is stirred for a predetermined time, and uniform slurry is prepared. Thereafter, when the pump 113 is driven such 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, and is discharged into the first column 12 from the seventh pipe L7 through the pipes, the pump, and the valves. Herein, the seventh pipe L7 allows the slurry to flow from an upper side with respect to a filling completion position of the filler in the first column 12. Consequently, the slurry in the tank 111 is transferred to the first column 12. Additionally, 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. Consequently, pressure rise in the first column 12, and pressure drop in the tank 111 are offset, slurry in the tank 111 are smoothly transferred to the first column 12, and a first column 12 is filled with the slurry.
Step S25 is a process of settling the filler in the first column 12. Hereinafter, Step S25 will be described with reference to
As described above, in a conventional technology, as filler is settled in the column, the thickness of the filler is increased, so that liquid is unlikely to be transmitted through layers of the filler, resistance against injection of the slurry into the column increases, and the injection speed of the slurry reduces. Consequently, there is a risk that the inside of the pipe is blocked by the filler. However, according to this embodiment, slurry that circulates through the tank 111 and the first column 12 does not transmit the settled filler, and slurry that flows out from the first column 12 through the ninth pipe L9 is supernatant liquid of the slurry in the first column 12, and therefore the concentration thereof is concentration previously adjusted in the tank 111, or less. Accordingly, the flow speed of the slurry in the pipe is not reduced, the slurry always flows, and the inside of the pipe is not blocked by the filler.
Step S26 is a process of optimally compressing and filling the filler in the first column 12. In this process, the pipes, the pump, and the valves are connected in a manner similar to Step S25. It is confirmed that substantially all the filler in the tank 111 is settled in the first column 12, and thereafter the fifth valve V5 is closed. Then, the lid 122 is detached from the first column tube 121, an adapter (not illustrated) is mounted on the first column tube 121. The adapter is mounted, so that the filler in the first column tube 121 is compressed at a predetermined compress ratio. Consequently, the filler is filled in the first column 12. The compress ratio of the filler is predetermined for each filler.
In Step S27, the first column 12 is used for chromatography.
The first column 12 is used for chromatography, and thereafter the filler in the first column is recovered to be reused. Hereinafter, processes of recovering the filler from the first column 12 in Steps S28 and S29 will be described with reference to
The process of recovering the filler from the first column 12 according to Step S28 has three different processes. Hereinafter, each process will be described.
First, a first recovery process will be described with reference to
First, when the pump 113 is driven such 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 118 with a filter to the fifth pipe L5, and is discharged into the first column 12 from the seventh pipe L7 through the pipes, the pump, and the valves. Consequently, the liquid in the tank 111 is transferred to the first column 12. The transferred liquid breaks and fluidizes the filler filled in the first column 12. 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. Herein, as described above, the leading end of the seventh pipe L7 is provided in such a shape and such a position that the discharged liquid swirls inside the first column tube 121. Therefore, the liquid can efficiently break and fluidize the filler.
When the first recovery process is started, setting is performed such that the second valve V2 opens the path between the fourth pipe L4 and the third pipe L3, and closes the path between the fourth pipe L4 and the third pipe L3, and the sixth pipe L6, and the pump 113 is driven such that the slurry flows from the third pipe L3 to the second pipe L2. Consequently, liquid in the resin bottle 114 is transferred to the tank 111 through the fourth pipe L4. In the first recovery process, the filler in the tank 111 is recovered by use of this liquid.
Now, a second recovery process will be described with reference to
First, when the pump 113 is driven such 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 118 with a filter to the fifth pipe L5, and is discharged into the first column 12 from the seventh pipe L7 and a bottom of the first column tube 121 through the pipes, the pump, and the valves. Consequently, the liquid in the tank 111 is transferred to the first column 12. The transferred liquid breaks and fluidizes the filler filled in the first column 12. 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. Herein, the liquid that flows from the bottom of the first column tube 121 can break the filler from the bottom, and fluidize the filler. Additionally, the liquid discharged from the leading end of the seventh pipe L7 flows so as to swirl in the first column tube 121, and can break and fluidize the filler. The liquid is injected from the two directions, so that the filler can be efficiently broken and fluidized to be recovered.
Now, a third recovery process will be described with reference to
Consequently, the suction port 117 is connected to the discharge port 116 through 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, the pipes, the pump, and the valves from the suction port 117 to the discharge port 116 are filled with liquid composing slurry. In this state, when the pump 113 is driven such 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, and is discharged into the first column tube 121 from the discharge port 116 through the pipes, the pump, and the valves. The filler in the first column tube 121 is stirred together with the liquid by flow of the discharged liquid. When this process is continued for a predetermined time, the filler and the liquid are mixed to produce slurry. Then, in a manner similar to Step S22, the slurry is transferred into the tank 1, and recovered.
In Step S29, the filler recovered in the tank 111 is discarded, or recovered and stored in the resin bottle 114. When the filler is recovered in the resin bottle 114, the first valve V1 opens the path between the first pipe L1 and the second pipe L2, and closes a path between the first pipe L1 and the second pipe L2, and the fifth pipe L5. Additionally, 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 driven such that the liquid flows from the second pipe L2 to the third pipe L3 while the stirring bar 112b is rotated, and the slurry stored in the tank 111 is stirred, the slurry in the tank 111 is sucked from the first pipe L1, and discharged into the resin bottle 114 from the discharge port 116 through the pipes, the pump, and the valves, and is recovered.
According to this embodiment, slurry can be stably transferred to the first column 12 without allowing the filler to stick to the inside of each pipe, and reducing the flow speed of the slurry in each pipe, or blocking the pipes by the slurry.
In Step S23 of the column processing method, in place of the scale, other measuring instrument or the like may be provided in the tank 111, and the volume of filler may be measured by use of the measuring instrument or the like. In Step S24, the fifth valve V5 may be opened. Consequently, the liquid in the first column 12 is transmitted through the filter 123 to be discharged to the outside, and only the filler is stored in the first column 12.
In the first to third recovery processes, the stirring bar 112b may be suitably rotated to stir the slurry in the tank 111.
Now, a second column 22 according to a second embodiment will be described with reference to
The adapter pipe 224 is a cylindrical member having the same outer diameter and inner diameter as the second column 22, and has pipe mounting ports being two through holes in a side surface. The seventh pipe L7 and the ninth pipe L9 are connected to the respective pipe mounting ports through two-way valves V3-1 and V4-1. The adapter pipe 224 is coaxially mounted on a top of the second column 22. In this state, a leading end of the seventh pipe L7 penetrates the side surface to reach an inner circumferential surface from an outer part of the second column 22, but does not protrude inward, and is provided in such a shape and such a position that slurry discharged from the leading end swirls inside the second column tube 221 (refer to
The lid 222 is made of disk-like resin or metal, includes a hole penetrating along the central axis, and is mounted on a top opening of the second column tube 221. An adapter 223 includes a piston 223a and an inlet pipe 223b. The piston 223a is made of disk-like resin or metal having such size as to enable engagement with the inner circumferential surface of the second column tube 221, and includes a hole axially penetrating along the central axis. The inlet pipe 223b is made of cylindrical resin or metal, and is connected to the piston 223a such that the hole of the piston 223a and an inner circumference of the inlet pipe 223b are connected. The inlet pipe 223b is slidably inserted into the through hole provided in the lid 222. In a state in which the lid 222 is mounted on the second column tube 221, the piston 223a can be moved axially in the second column tube 221 by axial movement of the inlet pipe 223b. As described above, the leading end of the seventh pipe L7 does not protrude inside the second column 22, and therefore the piston 223a can move from the axial end near the filling completion position of the second column tube 221 to a position beyond the filling completion position.
When the piston 223a moves to the vicinity of the lid 222, the seventh pipe L7 and the ninth pipe L9 are connected to a filler filling region 221a in the second column tube 221. In this state, slurry can be filled or recovered in the second column tube 221 through the seventh pipe L7 and the ninth pipe L9. On the other hand, when the piston 223a is moved into the filler filling region 221a, the piston 223a compresses the filler. Consequently, the filler is filled in the second column 22. At this time, the seventh pipe L7 and the ninth pipe L9 are disconnected from the filler filling region 221a.
In Steps S21 to S25, S27, and S29 in the column processing method, the piston 223a is moved to the vicinity of the lid 222, so that the second column 22 can be used in a manner similar to the first embodiment. Description of these steps will be omitted. In Step S26 of the column processing method, the piston 223a is moved into the filler filling region 221a without detaching the lid 222. Consequently, the filler is compressed up to a predetermined compress ratio by the piston 223a, and the filler is filled in the second column 22.
As to a connection state between the seventh pipe L7 and the ninth pipe L9, and the second column 22, an example of the connection state different from
This embodiment obtains the same effects as the first embodiment. Additionally, it is possible to fill the filler in the second column 22 without detaching the lid 222.
In
In any embodiment, two-way valves may be used in place of three-way valves. At this time, the single two-way valve can be provided in each pipe.
The first column tube 121 and the second column tube 221 may not be made of resin, and all or a part of each of the first column tube 121 and the second column tube 221 may be made of a metal material or a glass material.
The outer diameter of the filter 123 may be substantially the same as the inner diameters of the first column tube 121 and the second column tube 221. In this case, the outer diameter of the filter 123 only needs to be such a length as to block at least a hole formed by opening in the inner part of each of the first column tube 121 and the second column tube 221 by the fifth valve V5, and is preferably closer to the inner diameters of the first column tube 121 and the second column tube 221. The outer diameter of the filter 123 may be provided so as to be embedded with respect to the axial direction in a member forming a bottom of each of the first column tube 121 and the second column tube 221.
The stirrer 112 may not be a stirrer that does not include the stirring bar 112b mounted on the leading end of a rotary shaft 112a, and may be a magnetic type stirrer. In this case, a magnetized stirring bar is disposed in the tank 111, and is rotated by magnetic force through a wall of the tank 111. Consequently the stirring bar stirs slurry.
The leading end of the seventh pipe L7 may not be provided in such a shape and such a position as to form swirl, or may be a linear shape. Additionally, the leading end of the seventh pipe L7 may not protrude to the inner part of the first column 12, and may be provided so as to penetrate the lid 122 up to such a position as to be substantially flush with a surface inside the first column 12 in the lid 122.
In Step S25, the sixth valve V6 may be opened or blocked. As described above, the sixth valve V6 is installed on the upper side in the gravity direction with respect to the first column 12. Therefore, the sixth valve V6 is opened, so that atmospheric pressure is applied to the inside of the first column 12 through the tenth pipe L10 and the ninth pipe L9. Consequently, discharge of liquid from the fifth valve V5 is facilitated. Therefore, the sixth valve V6 is opened or blocked, so that it is possible to adjust a reflux speed of slurry from the first column 12 to the tank 111. At this time, the sixth valve V6 is opened or blocked so that the slurry does not jet from the eleventh pipe L11. Alternatively, in a case where the inner diameter of the pipe extending from the sixth valve V6 to the inside of the tank 111 has such a size as not to interrupt reflux of the slurry, it is estimated that the slurry does not jet from the eleventh pipe L11, and therefore the sixth valve V6 can be normally opened, or omitted.
Now, Examples 1 to 3 according to the first and second embodiments will be indicated, and the effects of the first and second embodiments will be described. The technical scope of the present invention is not limited by these examples at all.
(1) Steps S23 to S27 were implemented as described below by using a configuration illustrated in
A filler over column volume and pure water were mixed in a tank, and slurry whose concentration was 50 vol % was prepared.
A A column was assembled, and pure water was filled in a column from a bottom in order to prevent bubbles from entering the column.
B A lid composed of a silicon plug for filling was mounted on a top opening of the column.
C As illustrated in
D Slurry was stirred by a stirrer.
E The pump was activated, and the slurry was fed into the column.
A fifth valve V5 was opened after feeding, an accumulating speed of the filler, and a draining amount from a column lower part were checked until the settling height of the filler in the column reaches 45 cm (90% of column volume).
The adapter was mounted on the top opening of the column, and the filler was compressed in the vertical direction.
A filling state was evaluated by chromatographic analysis. An evaluation condition by the chromatographic analysis is as follows:
Herein, the “Revolution Number of Stirring” is the revolution number of the stirrer, and the “Revolution Number of Pump” is the revolution number of the pump. Additionally, the “Draining-Slurry Recovering Height Difference” is a distance from a slurry surface in the tank to a liquid level at which liquid is discharged from a tank bottom to the outside. The “Feeding Amount (After Filling)” is an amount of feeding slurry to the column in a period during which slurry is filled in the column. The “Slurry Concentration (After Filling)” is the concentration of slurry that remains in the tank 111 after filling of slurry into the column is completed.
Now, an evaluation result is listed.
The settling height of the filler in the column is listed in Table 2.
Time change of an draining amount from the fifth valve is illustrated in
The chromatography resulted in one mountain having excellent symmetry, and in excellent number of theoretical plates.
A distance from a slurry surface in the tank 111 to a liquid level at which liquid is discharged from a tank bottom to the outside is set to 16.5 cm, 21.5 cm, and 44.5 cm, and a flow-out liquid amount per unit time from a column bottom was measured by a graduated cylinder in a state in which resin of about 7 cm (70% of column volume) was settled in a column having an inner diameter of 1 cm, a pipe height of 10.6 cm, capacity of 0.79 cm2, and column volume (CV) of 8.4 mL, and in a state in which remaining slurry of 20% is circulated, and the flow-out speed was obtained.
The evaluation result is listed. The flow-out speed in a case in which the distance was set to 16.5 cm was 0.38 mL/min, the flow-out speed in a case in which the distance was set to 21.5 cm was 0.45 mL/min, and the flow-out speed in a case in which the distance was set to 44.5 cm was 0.75 mL/min. It was confirmed that the longer the distance from the slurry surface in the tank 111 to the liquid level at which the liquid is discharged from the tank bottom to the outside was, that is, the higher the water head was, the faster the flow-out speed was.
A distance from a slurry surface in the tank 111 to a liquid level at which liquid is discharged from a tank bottom to the outside is set to 16.5 cm, slurry of 15.2 mL containing resin having column volume (CV) of 90% (7.6 mL) was circulated in a column having an inner diameter of 1 cm, a pipe height of 10.6 cm, capacity of 0.79 cm2, and column volume (CV) of 8.4 mL, and an amount of a filler settled inside a column was measured.
The evaluation result is listed. The amount of the settled filler was 70%. The resin could be transferred to the column without blocking pipes by slurry, and settled into the column.
The sizes of the respective members described in this specification and illustrated in the drawings are an example, and the present invention is not limited to these sizes. Additionally, materials of the respective members are an example, and the present invention is not limited to these materials.
Although the embodiment of the present invention is described with reference to the accompanying drawings, it will be obvious to those skilled in the art that a structure and relation of each component may be modified within the scope and spirit of the present invention described herein.
| Number | Date | Country | Kind |
|---|---|---|---|
| 2018-110250 | Jun 2018 | JP | national |
