JP2013160526A - Chromatographic column and movable plug therefor - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a movable plug for a chromatographic column in which the movable plug can be moved smoothly without leaking a liquid or filling agent by performing fine adjustment on a sealing strength in spite of a simple structure.SOLUTION: A movable plug comprises a movable plug core, a scraper, a base, packing and drawing means. The drawing means includes a bolt which is screwed through the base to the movable plug core and a disc spring interposed between a head of the bolt and the base. Furthermore, it is preferable that a tightening torque of the bolt is 1 to 40 N m.

Description

  The present invention relates to a movable stopper used in a column for liquid chromatography (chromatography column), and a chromatography column using the movable stopper.

  Liquid chromatography is widely used as a means for separating and purifying a target substance in a natural product, a fermentation product, a cultured product obtained by gene recombination, or a synthetic reaction product at a desired purity and purification rate.

  Conventionally, packing of a packing material into a column for liquid chromatography is performed by a method as shown in FIGS.

  That is, the liquid chromatography column 21 shown in FIG. A slurry 23 prepared by mixing a filler with a solvent as shown in FIG. Then, as shown in FIG. 3 (c), an upper cover 24 having a solvent outlet (not shown) at the top of the column 21 and provided with a porous plate for preventing the outflow of the filler is attached, and the movable stopper 22 is pushed up. Thus, the solvent is pushed out from the solvent outlet of the upper lid 24, and as shown in FIG. 3D, the filler filling layer 25 is formed under pressure. That is, by moving the movable stopper 22, a uniform filling layer is laminated from the side opposite to the movable stopper, and after the filling is completed, the pressure of the filling layer 25 by the movable stopper 22 is maintained. This packing apparatus is widely known as an axial compression type column. A seal structure is provided between the inner peripheral surface of the column 21 and the movable stopper 22 so that the liquid and the filler are prevented from leaking tightly.

  As such a sealing structure between the inner peripheral surface of the column 21 and the movable stopper 22, for example, an O-ring packing or a structure in which compressed air is removed after the movable stopper has moved to a predetermined position (patented) Reference 1). Patent Document 2 discloses the use of packing having a substantially V-shaped cross section (V packing).

Japanese Patent No. 4098342 JP 2011-191256 A

  The sealing force when sealing between the inner peripheral surface of the column and the movable stopper by packing is determined by how much the packing is crushed, but it can be used for changes in elasticity due to deterioration of the packing and movement of the movable stopper. Along with this, the sealing force changes over time due to changes in the outer diameter of the packing and the inner diameter of the column due to friction generated between the movable stopper and the inner peripheral surface of the column. Further, the sealing force varies depending on the degree of cleaning of the packing and the inner wall surface of the column. In other words, in order to keep the sealing force constant and to operate the sealing mechanism safely, there is a problem that management and work for constantly checking the state of the packing and the column and performing cleaning and replacement are necessary.

  Further, the seal structure described in Patent Document 1 is pressurized with a compression medium, the seal portion is retracted and loosened, the movable stopper is moved to a predetermined position in the column, and then the compression with the compression medium is performed. Except for this, the sealing material is pressed and sealed by the pressing force of the spring. In this method, since the pressing force of the spring changes depending on the elapsed time due to the deterioration of the spring repulsive force, it is still difficult to maintain a certain sealing accuracy, and the filler slurry enters between the seal portion and the inner wall surface of the column. In order to prevent this, when the movable stopper is moved with little or no loosening of the seal, there is a problem that the movement of the movable stopper is not easy. Moreover, due to the severe wear of the seal material, the life of the seal material is shortened and it is necessary to replace it frequently. However, it is not easy to predict the replacement time, and the time, labor, and cost of the seal material required for replacement There are also problems such as being costly and not economical.

  Further, in the seal structure described in Patent Document 2, the V packing expands in the diameter-expanding direction by a bolt or a screw structure provided on the movable plug core and the base, so that the inside of the movable plug and the column is expanded. Although sealing with the peripheral surface is performed, even in this method, when the movable stopper is moved without loosening or hardly loosening, there is a problem that the movable stopper is not easily moved.

  The present invention solves the above-mentioned conventional problems, and has a simple structure, but by adjusting the sealing force finely, a chromatographic column that enables a smooth movement of the movable stopper without leaking liquid or packing material. An object of the present invention is to provide a movable stopper. Another object of the present invention is to provide a liquid chromatography column provided with this movable stopper.

  In order to solve the above problems, first, the present invention relates to a movable stopper disposed in a column of liquid chromatography, the tip of the movable stopper faces the packing material, and the axial center of the movable stopper is the axial center line of the column. A movable stopper core extending in the direction, an annular scraper externally fitted to the outer periphery of the distal end side of the movable stopper core, a base having a recess in which a proximal end side of the movable stopper core is internally fitted, and the scraper and the base A packing surrounding the outer periphery of the movable plug core, and a pulling means for pulling the movable plug core in a direction of pushing the movable plug core into the recess of the base. There is provided a movable plug comprising: a bolt that penetrates a base and is screwed to the movable plug core; and a disc spring interposed between the head of the bolt and the base (Invention 1). ).

  According to this invention (Invention 1), when the movable stopper is moved with little or no loosening of the seal, the repulsive force acting on the packing from the column inner peripheral surface is absorbed not only by the packing itself but also by the disc spring. Thus, the frictional force between the packing and the inner circumferential surface of the column can be finely adjusted, so that the movable stopper can be smoothly moved in the column.

  In the said invention (invention 1), it is preferable that the bolt tightening torque is 1 to 40 N · m (invention 2).

  According to this invention (invention 2), it is possible to realize an operation in which the movable stopper moves smoothly without leaking liquid or filler.

  A second aspect of the present invention provides a liquid chromatography column (Invention 3), in which the movable stopper of the above inventions (Inventions 1 and 2) is disposed inside.

  According to this invention (Invention 3), the movable stopper as described above is arranged in the column of the liquid chromatography, and the packing is expanded in the diameter increasing direction by pressing the movable stopper. When the packing comes into contact with the inner peripheral surface of the column, the seal between the movable stopper and the inner peripheral surface of the column is performed. At this time, when the movable stopper is moved with little or no loosening of the seal, the repelling force acting on the packing from the inner peripheral surface of the column is absorbed not only by the packing itself but also by the disc spring, thereby Since the frictional force with the surface can be finely adjusted, smooth movement of the movable stopper in the column can be realized without leaking liquid or packing material.

  The movable stopper of the present invention and the chromatographic column equipped with this movable stopper have a simple structure, but fine adjustment of the sealing force realizes smooth movement of the movable stopper without leaking liquid or packing material. can do.

It is a longitudinal section showing a movable stopper concerning one embodiment of the present invention. It is a longitudinal cross-sectional view which shows the movable stopper which concerns on another one Embodiment of this invention. It is a longitudinal cross-sectional view which shows a prior art example schematically.

  Hereinafter, embodiments will be described with reference to the drawings.

[First Embodiment]
First, the first embodiment will be described. FIG. 1 is a longitudinal sectional view in the axial direction showing a movable stopper according to an embodiment of the present invention.

  The movable stopper 1 of the present embodiment includes a movable stopper core 2, a scraper 3, a base 4, and a V packing 5, and the tip side (the upper end side in the figure) is in contact with the packing material in the column (not shown). Are arranged as follows. The movable plug core 2 is formed of a substantially cylindrical body that extends in the axial direction from the distal end of the movable plug 1. From the middle of the movable plug core 2 to the base end side (the lower end side in the figure), a cylindrical portion having an equal diameter is formed, and the upper side of the cylindrical portion is a flange portion 6.

  The lower surface of the flange portion 6 is a tapered surface 6a whose diameter increases toward the top. A shallow circular recess 7 is provided on the upper end surface of the movable plug core 2, and a diameter-expanded step portion 8 is formed on the upper side of the side peripheral surface of the recess 7. By engaging the stepped portion 8, the porous plate 9 is attached to the distal end surface of the movable plug core 2, and the liquid is distributed and supplied or collected and discharged between the porous plate 9 and the bottom surface of the recess 7. A vacant chamber S is formed. A communication hole 10 for supplying or discharging liquid is formed so as to penetrate from the center of the bottom surface of the recess 7 to the center of the bottom surface of the movable plug core 2. A female screw hole 11 into which a pressing bolt 12 as a pulling means is screwed is formed on the bottom surface of the movable plug core 2 in a direction parallel to the axis of the movable plug 1. 12 a is a disc spring interposed between the head of the pressing bolt 12 and the base 4.

  The scraper 3 is an annular member fitted to the outer periphery of the flange portion 6. The outer peripheral surface of the scraper 3 is a cylindrical surface having an equal diameter. The inner peripheral surface of the scraper 3 is a tapered surface 13 that overlaps the tapered surface 6a. The bottom surface of the scraper 3 is perpendicular to the axis of the movable stopper 1.

  The base 4 has a substantially cylindrical shape, and a recess 14 into which the lower portion of the movable plug core 2 is fitted is provided at the center of the upper surface. A liquid flow hole 15 that penetrates from the bottom surface of the recess 14 to the bottom surface of the base 4. Is formed. Further, an insertion hole 16 for the pressing bolt 12 is formed so as to penetrate from the bottom surface of the recess 14 to the bottom surface of the base 4.

  A plurality of V packings 5 are arranged in a stacked manner between the scraper 3 and the base 4, and have an annular shape that circulates around the movable plug core 2. An upper pedestal 17 and a lower pedestal 18 are interposed between the laminated body of the V packing 5 and the scraper 3 and between the laminated body and the base 4, respectively.

  The V packing 5 has a predetermined thickness and width, and has a V-shaped groove angle and a V-shaped apex angle, and the groove angle is smaller than the apex angle. Further, the upper pedestal 17 of the V packing 5 has a predetermined thickness, the same width as the V packing 5, and the same apex angle as the V packing 5. Furthermore, the lower pedestal 18 of the V packing 5 has a predetermined thickness, the same width as the V packing 5, and the same groove angle as the V packing 5. By making the groove angles of the V packing 5, the upper pedestal 17 and the lower pedestal 18 smaller than the apex angle, a plurality of V packings 5 are stacked between the upper pedestal 17 and the lower pedestal 18, and the axial direction (the vertical direction in the figure). ), The V packing 5 is likely to spread outward, so that not only the sealing performance between the movable stopper core 2 and the scraper 3 is improved, but also the sealing performance between the V packings 5 adjacent to each other in the vertical direction. Will also improve.

  The pressing bolt 12 is screwed into the female screw hole 11 through the insertion hole 16. After the disc spring 12a of the pressing bolt 12 comes into contact with the bottom surface of the base 4, by further rotating the pressing bolt 12, the movable plug core 2 is attracted to the base 4 side, and the V packing 5 is connected to the scraper 3 and the base. 4 and is expanded in the diameter increasing direction. When the V packing 5 comes into contact with the inner peripheral surface of a chromatography column (not shown), the movable stopper 1 and the inner peripheral surface of the column are sealed. The tightening torque of the pressing bolt 12 is preferably 1 to 40 N · m, particularly 2 to 30 N · m so that the movable stopper can move smoothly without leaking liquid or filler.

  The disc spring 12a has the effect of finely adjusting the force that attracts the movable plug core 2 by the pressing bolt 12 to the base 4 side. Accordingly, when the movable stopper 1 is moved in the column in a state where the movable stopper 1 and the inner peripheral surface of the column are sealed, the movable stopper 1 acts on the V packing 5 from the inner peripheral surface of the column. The repulsive force can be absorbed not only by the V packing 5 itself but also by the disc spring 12a. As a result, the frictional force generated between the V packing 5 and the inner peripheral surface of the column can be finely adjusted, so that the movable stopper can be smoothly moved in the column.

  In the movable stopper 1 having such a configuration, the scraper 3 is a non-rigid body (non-metal), and the outer diameter of the scraper 3 before inserting the column is equal to or slightly larger than the inner diameter of the column. The outer peripheral surface of the scraper 3 is preferably pressed against the inner peripheral surface of the column. Examples of the material of the scraper 3 include fluorinated resins such as polytetrafluoroethylene and partially fluorinated resins such as polychlorotrifluoroethylene, polyvinylidene fluoride, polyvinyl fluoride and fluorinated resin copolymers, For example, a perfluoroalkoxy fluororesin, a tetrafluoroethylene-hexafluoropropylene copolymer, an ethylene-tetrafluorinated ethylene copolymer, and the like are preferable. In addition to these, fluorinated resin, partially fluorinated resin, rubber coated with a fluorinated resin copolymer, fluororubber, EPDM, and the like are also applicable.

  The material of the movable plug core 2 is preferably a corrosion-resistant metal such as stainless steel, titanium, or hastelloy, but may be a synthetic resin such as fluororesin, polypropylene, polyethylene, polysulfone, acrylic, or methylpentene.

  A preferable material of the base 4 is exemplified by the same material as that of the movable plug core 2, but is not limited thereto. The outer diameter of the base 4 is preferably smaller than the inner diameter of the column, and is preferably at least an intermediate value between the inner diameter and the outer diameter of the lower pedestal 18.

  The number of stacked V packings 5 is preferably 2 or more, particularly about 2 to 4 sheets. The material of the V packing 5 is natural rubber, EPDM, polytetrafluoroethylene, tetrafluoroethylene / perfluoroalkyl vinyl ether copolymer, tetrafluoroethylene / hexafluoropropylene copolymer, tetrafluoroethylene / ethylene copolymer, Polyvinylidene fluoride, polychlorotrifluoroethylene, Teflon (registered trademark) -coated rubber, and the like are suitable, but not limited thereto.

  As a material of the disc spring 12a, a generally used material from a soft material to a hard material can be applied according to the magnitude of pressure to be adjusted. The thickness and size of the disc springs 12a, the number of sheets to be overlapped, and the like can be arbitrarily selected according to the magnitude of the pressure to be adjusted.

  In the movable plug 1 as described above, the V packing 5, the upper pedestal 17 and the lower pedestal 18 have the same width, and the groove angle is smaller than the apex angle. The peripheral portions of the adjacent members are in close contact with each other, while a gap is generated between the bottom of the groove angle and the top of the apex angle. When the pressing bolt 12 is screwed in here, the base 4 is attracted upward, and the interval between the upper base 17 and the lower base 18 is reduced, whereby the V packing 5 is pressed. At this time, as described above, there is a gap between the bottom of the adjacent groove angle and the top of the apex angle, so that the V-packing 5 is easily expanded outward and pressed against the inner wall surface of the column. The sealing performance by the V packing 5 itself can be improved.

  Then, the movable plug core 2 is attracted to the base 4 side using the pressing bolt 12 and the disc spring 12a, and the V packing 5 is expanded in the diameter increasing direction to seal the movable plug 1 and the inner peripheral surface of the column. Therefore, when the movable stopper 1 is moved in the column in a state where the movable stopper 1 and the inner peripheral surface of the column are sealed, smooth movement of the movable stopper 1 can be realized. it can. Furthermore, in this embodiment, the sealing performance of the V packing 5 can be easily adjusted by inserting and removing the pressing bolt 12 and adjusting the screwing pressure (torque). Moreover, the movable plug 1 of the present embodiment can easily replace the V packing 5 by removing the pressing bolt 12 and separating the base 4 and the movable plug core 2.

[Second Embodiment]
Next, a second embodiment will be described. FIG. 2 is a longitudinal sectional view in the axial direction showing a movable stopper according to another embodiment of the present invention.

  As shown in FIG. 2, the movable plug 1A according to the present embodiment uses an O-ring 50 as a packing instead of the V packing 5, the upper pedestal 17 and the lower pedestal 18 in the movable plug 1 according to the first embodiment. It was. Since all other configurations are the same as those of the movable stopper 1 according to the first embodiment, detailed description thereof is omitted.

  Materials for the O-ring 50 include natural rubber, EPDM, polytetrafluoroethylene, tetrafluoroethylene / perfluoroalkyl vinyl ether copolymer, tetrafluoroethylene / hexafluoropropylene copolymer, tetrafluoroethylene / ethylene copolymer, Polyvinylidene fluoride, polychlorotrifluoroethylene, Teflon (registered trademark) -coated rubber, and the like are suitable, but not limited thereto.

  Also in this embodiment, after the disc spring 12a of the pressing bolt 12 comes into contact with the bottom surface of the base 4, by further rotating the pressing bolt 12, the movable plug core 2 is attracted to the base 4 side and the O-ring. 50 is pinched between the scraper 3 and the base 4 and expands in the diameter increasing direction. The O-ring 50 comes into contact with the inner peripheral surface of a chromatography column (not shown), thereby sealing the movable stopper 1A and the inner peripheral surface of the column.

  Further, the disc spring 12a has an effect of finely adjusting the force of the movable plug core 2 by the pressing bolt 12 to attract the base 4 side. Thus, when the movable stopper 1A is moved in the column in a state where the movable stopper 1A and the inner peripheral surface of the column are sealed, the movable stopper 1A acts on the O-ring 50 from the inner peripheral surface of the column. The repulsive force can be absorbed not only by the O-ring 50 itself but also by the disc spring 12a. As a result, the frictional force generated between the O-ring 50 and the inner peripheral surface of the column can be finely adjusted, so that the movable stopper can be smoothly moved in the column.

  The present invention has been described above with reference to the accompanying drawings, but the present invention is not limited to the above-described embodiment, and various modifications can be made.

  Since the chromatographic column using the movable stopper of the present invention as described above has no leakage of liquid or filler, the chromatographic separation and purification efficiency can be increased. Liquid chromatography using such a chromatographic column is suitable as a means for separating and purifying target substances in natural products, fermented products, cultured products by genetic recombination, etc., and synthetic reaction products at the desired purity and purification rate. is there.

DESCRIPTION OF SYMBOLS 1, 1A ... Movable stopper 2 ... Movable stopper core 3 ... Scraper 4 ... Base 5 ... V packing 50 ... O-ring 7 ... Recess 12 ... Pressing bolt (attraction means)
12a ... disc spring

Claims (3)

In a movable stopper placed in a liquid chromatography column,
A movable plug core with the tip facing the packing material and extending the axial center of the movable plug in the axial direction of the column;
An annular scraper fitted around the outer periphery of the distal end side of the movable plug core;
A base having a recess in which the proximal end side of the movable plug core is fitted,
A packing surrounding the outer periphery of the movable plug core between the scraper and the base;
A pulling means for pulling the movable plug core in a direction of pushing into the recess of the base;
The movable means characterized in that the attraction means comprises a bolt that penetrates the base and is screwed to the movable stopper core, and a disc spring interposed between the head of the bolt and the base. plug.   The movable stopper according to claim 1, wherein a tightening torque of the bolt is 1 to 40 N · m.   A liquid chromatography column, wherein the movable stopper according to claim 1 or 2 is disposed therein.

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