CN86203547U - Centrifugal countercurrent chromatograph with end face rotary seal - Google Patents

Abstract

The utility model designs a centrifugal countercurrent chromatograph with end face rotary sealing, which has a countercurrent chromatographic rotor on which a spiral capillary is wound. Rotary seals are used between the rotor and the centrifuge cover instead of planetary transmission. Therefore, not only the essence of the Ito-type countercurrent chromatograph is maintained, but also its mechanical structure is simplified. The chromatograph can not only run on a special centrifuge, but can also be used as an accessory on a laboratory centrifuge, which is easy to popularize and use.

Description

The utility model belongs to the improvement of a countercurrent chromatograph.

The Ito-type countercurrent chromatography technology invented by Ito Yoichiro is the same as the general liquid chromatography technology. In addition to the characteristics of continuous sampling and detection, it also has its unique characteristics, that is, the Ito-type chromatograph does not use solid supports ( Packing agent) liquid column chromatography, the helical capillary is equivalent to chromatography (chromatographic) column. Due to the absence of sample loss on the packing, this technique results in reproducible and pure component separations.

The Ito type chromatograph (Yoichiro Ito, Journal of Bioche-mical and Biophysical Methods, 5, 1981, P105-P129) has a rotating drum on which a helical capillary is wound. After the soft capillary is first wound on the thin core rod, the thin core rod is wound on the rotating drum. It is also possible to wind the thin stamen rods on several thicker stamen rods, and connect them together properly on the drum. The drum runs on a planetary centrifuge, that is, the drum also revolves in addition to rotation, resulting in a changing centrifugal force. There is a specific relationship between the rotation speed and the rotation direction and the revolution, thus avoiding the twisting of the inlet and outlet hoses and realizing the free passage of liquid. The planetary motion is realized by a series of gears and belt drives, and the structure is complex.

The Ito-type chromatograph is mainly used in his laboratory, mainly used in a few laboratories in the United States, and has been produced by the American P.C.INC. company.

The Ito-type chromatograph can only be realized on a dedicated planetary centrifuge. If it is to be realized on any commodity laboratory centrifuge, it must try to adopt a planetary drive (Ito, U.S. Patent 4,182,678, August 1980; Ito, U.S. Patent 3,994,805, November 1976; I, A, Sutherland, etc., Journal of Liquid Chro-matography, 7(2), 363-384, 1984), therefore, the further promotion of the Ito-type chromatograph is subject to Limitations of its complex mechanical structure.

The utility model designs a centrifugal countercurrent chromatograph, which has a centrifugal rotor surrounded by a spiral capillary, and adopts end face rotary sealing instead of planetary transmission. Therefore, not only the essence of Ito type countercurrent chromatography is maintained, but also its mechanical structure is greatly simplified. The system can not only run on a special centrifuge, but also run on a common laboratory centrifuge, which is suitable for popularization and use.

In the countercurrent chromatograph designed by the utility model, the centrifugal force generated by the rotation of the centrifugal rotor is proportional to the square of the rotating speed and the radius of the rotor. When the solution to be separated flows through the helical tube wound on the rotor, Ito type countercurrent chromatographic separation occurs. The end face rotary seal is adopted in the liquid inlet and outlet mechanism of the spiral tube, which avoids twisting of the inlet and outlet hoses, and realizes the simplification of the existing Ito type chromatograph.

The centrifugal countercurrent chromatograph with end-face rotary seal proposed by the utility model includes a driver (1), a shaft sleeve (2), a centrifugal chromatographic rotor, a spiral capillary (4) wound on the rotor, an end-face rotary seal mechanism, and a centrifugal cavity ( 6] and cover [7].

The utility model is characterized in that the rotation of the centrifugal chromatographic rotor is not planetary motion, but simple rotation. In order to prevent the twisting of the liquid inlet and outlet pipes, an end face rotary sealing mechanism is used between the centrifuge chromatographic rotor and the centrifuge cover. The centrifugal chromatographic rotor can be integrated, and its pair of lower ports of the liquid channel are connected with the inlet and outlet of the helical capillary. The end face rotary seal includes a dynamic seal, a static seal, a pressing force mechanism and a ball bearing unit each having a pair of liquid passages. The dynamic seal is installed on the upper part of the centrifugal chromatographic rotor, and the upper and lower ports of the dynamic seal liquid channel are respectively connected with the static seal and the liquid channel of the centrifugal chromatographic rotor. The static seal is installed at the lower part of the pressing force mechanism, and the bottom of the static seal is in contact with the top of the dynamic seal to form a friction surface. The ball bearing unit is connected with the centrifugal chromatographic rotor and the pressing force mechanism, and the cover is connected with the pressing force mechanism so that it does not rotate.

As mentioned above, the centrifugal chromatographic rotor can be made as a whole, but considering the manufacturing process, it can be composed of parts such as rotor body (3), rotating disk (5) and rotor core body (8). In order to keep the rotor stable in rotation, the rotor body, rotating disk and rotor core body can adopt garden cylinder or garden cone.

The lower end of the rotor body (3) is connected with the axle sleeve (2) to transmit power. The upper section of the rotor body is connected with the turntable to drive it to rotate.

Turning disk (5) is wound with helical capillary (4), for making the material flowing through helical capillary be subject to the centrifugal force as large as possible, the diameter of rotating disk is much larger than rotor body and rotor core body.

Rotor core body (8) is installed on the upper central part of rotor body (3) or rotating disk (5), rotates together with rotor body. A dynamic seal (12) is inlaid on the core body of the rotor, and has two passages connected with the liquid inlet and outlet passages of the dynamic seal. Connect the outer ring of ball bearing (31) at rotor pistil upper section.

The end face rotary sealing mechanism comprises a dynamic seal (12), a static seal (19), a pressing force mechanism and a ball bearing unit.

Dynamic seal (12) is inlaid on the garden shape concave surface of rotor pistil hole bottom.

Static seal (19) is embedded in support sleeve (20) bottom, and the other side contacts with the top of dynamic seal, forms the friction pair surface. Both the dynamic seal and the static seal have liquid inlet and outlet channels.

The pressing force mechanism comprises support sleeve (20), installation sleeve (28), elastic body (22) and pressing force adjustment assembly etc. Compression force adjustment assembly comprises mounting piece (24) and adjusting screw. Support sleeve (20) inside is divided into upper and lower two parts: elastic body (22) and adjustment screw (23) are housed in its upper part; Static seal is inlaid in its lower part. Support sleeve (20) is contained in the installation sleeve (28), can realize that support sleeve (20) can only move up and down in the installation sleeve (28) with simple mechanism such as available key and keyway, can not rotate. Mounting piece (24) is housed on installation sleeve (28) inside top, and its below is support sleeve (20). The installation part is in the installation sleeve (28), the change of its installation position and the change of the screwing degree of the adjustment screw in the installation part will cause the force change of the elastic body (22) to achieve the adjustment of the pressing force, thereby adjusting The tightness of the friction surface between the dynamic and static seals. As we all know, the friction surface should be finished to avoid liquid leakage during rotation, and the static seal is made of softer material and the dynamic seal is made of harder material.

The ball bearing unit is the connecting piece between the end face rotary sealing mechanism and the rotor core body, and it includes a ball bearing (31), a nut (21) and a pressing piece. The outer ring of ball bearing (31) cooperates with the inner garden cylinder on the top of the rotor pistil body, and the inner circle of ball bearing cooperates with the outer garden cylinder at the lower end of the installation sleeve (28). When the rotor rotates, the outer ring of the ball bearing rotates with the core body of the rotor, while the inner ring of the ball bearing stands still with the mounting sleeve. Therefore, the liquid inlet and outlet pipes (25, 26) (two capillaries) drawn from two transverse holes of static seal are not twisted in rotation. Mounting sleeve (28) hooks cover with a bent arm or with the structure that plays same effect, makes mounting sleeve not rotate when rotor rotates.

The inner diameter and length of the capillary are determined by the properties of the substance to be separated. Generally speaking, when separating small substances, a capillary with a small inner diameter and a long length is required. According to the needs, the inner diameter of the capillary is in the range of 0.2 to 5 mm, the diameter of the spiral winding is in the range of 1 to 20 mm, the number of spiral turns is in the range of tens to thousands, and the total length of the capillary is in the range of several to tens of meters. A set of numbers. Similarly, the diameter of the turntable can be 150-450 millimeters as required, and a set of numbers can be taken in the range of several hundred to 5000 rpm.

Axle sleeve (2) is fixed on the driver (1), and becomes integral rotation.

The shaft sleeve (2) is connected with the rotor body (3), transmits torque and drives the rotor to rotate.

The dynamic seal in the end face rotary seal mechanism rotates with the rotor while the static seal remains stationary.

The utility model has the advantages that it not only maintains the essence of the recently developed Ito-type chromatograph, that is, the countercurrent chromatographic capability of the rotating capillary in the centrifugal field, but also replaces the complex planetary transmission mechanism with an end face rotary sealing mechanism, so that The structure is greatly simplified. Therefore, the new chromatograph proposed by the utility model has strong practicability. It can be used not only on a special centrifuge, but also as a distribution rotor on an ordinary laboratory centrifuge, at this time, it only needs to be slightly modified on the original centrifuge cover. Therefore, the chromatograph is easy to popularize.

Fig. 1 is the chromatograph embodiment schematic diagram that the utility model proposes, wherein:

1. Driver; 2. Shaft sleeve; 3. Rotor body; 4. Spiral capillary; 5. Turntable; 6. Centrifugal chamber; 7. Cover; 8. Rotor body.

Figure 2 shows the end face rotary seal mechanism, where:

9. The central vertical hole of the rotor core body; 10. The transverse hole of the rotor core body; 11. The sealing ring; 12. The dynamic seal; 13. The liquid nozzle of the rotor core body; 14. The liquid outlet pipe of the rotor core body; 15. 16. Central vertical hole of static seal; 17. Liquid inlet nozzle of static seal; 18. Transverse hole of static seal; 19. Static seal; 20. Support sleeve; 21. Nut; 22. Elasticity Body; 23. Adjusting screw; 24. Installation piece; 25. Static seal liquid inlet pipe; 26. Static seal liquid outlet pipe; 27. Curved arm; 28. Mounting sleeve; 29. Spring card; 30. Pressure ring; 31 , ball bearing; 32, statically sealed horizontal hole; 33, statically sealed liquid outlet; 34, statically sealed eccentric vertical hole; 35, rotor core body liquid inlet pipe; 36, rotor core body liquid inlet nozzle; 37. The transverse hole of the rotor core body; 38. The sealing ring; 39. The eccentric vertical hole of the rotor core body;

An embodiment of the end-face rotary seal centrifugal countercurrent chromatograph proposed by the utility model is shown in FIG. 1 . It comprises a driver (1), a shaft sleeve (2), a rotor, a helical capillary (4) wound on the rotor, an end face rotary sealing mechanism, a centrifugal cavity (6) and a cover (7).

The rotor includes a rotor body (3), a rotating disk (5) and a rotor core body (8), and the three are fixedly connected to form an integral rotor to rotate. For the smooth rotation of the rotor, the installation of the three should ensure concentricity. The lower portion of the inner hole of the rotor body lower part has a tapered surface, which is matched with the corresponding tapered surface of the axle sleeve (2). The rotor runs on the shaft sleeve and can be removed from the shaft sleeve when not in use. Rotor body (3) top outer garden band protruding platform, rotating disk (5) is installed, fixes with screw. There is a hole in the center of the upper end of the rotor body (3), which is packed into the rotor core body (8) with an interference fit, and the rotor is made of aluminum alloy.

Turning disk (5) is a garden disk, and there is a garden hole in the center, is wound with helical capillary (4) on concave surface. The turntable is made of aluminum alloy with an outer diameter of φ300mm and a thickness of 22mm.

The spiral capillary adopts a plastic capillary tube with an outer diameter of φ1.8mm and an inner diameter of φ1.2mm, which is wound on an iron wire with an outer diameter of φ2.2mm and wound on the side of the turntable. The total number of spiral turns is about 400, and the total length of the capillary About 5.5 meters.

The rotor core body (8) is fixed on the center of the upper part of the rotor body (3) in an interference fit mode, and is made of stainless steel to prevent organic solvents from corroding the feeding channel. The rotor core body is a cylindrical body with an upward opening in the center. No through hole has a garden-shaped recess at its bottom as an inlaid dynamic seal (12). There is a central vertical hole (9) and an eccentric vertical hole (39) on the concave surface that cooperates with the dynamic seal, and the solid part of the lower part of the concave surface is connected to two transverse holes (37) leading to the inlet and outlet nozzles (36, 13). , 10) are connected. On the concave surface that contacts with dynamic seal, be processed with center vertical hole as the center, take the eccentric moment of eccentric vertical hole as an annular groove (40) of radius, and groove width is consistent with aperture. Make protruding ring or adorn spring clip to install ball bearing on the cylindrical surface in the inner body of rotor core, go out screw thread and nut (21) match in outer garden cylindrical surface upper part, be used for pressing down ball bearing.

The end face rotary sealing mechanism includes a dynamic seal (12), a static seal (19), a pressing force mechanism and a ball bearing unit (as shown in Figure 2). Dynamic seal (12) is to have a center vertical hole and the flat garden cylinder of an eccentric vertical hole. Its central vertical hole is aligned with the central vertical hole of the rotor core body. The eccentricity of the eccentric vertical hole is the same as the corresponding eccentricity of the rotor core body. The eccentric vertical hole needn't be aligned with the eccentric vertical hole of the rotor core body during assembly, and the annular groove (40) of the rotor core body connects the eccentric vertical holes of the two parts to form a liquid passage.

There are two sealing rings (11, 38) between the dynamic seal and the rotor core body, wherein the small ring (11) is around the central vertical hole, and the large ring (38) is on the outer periphery of the annular groove (40), preventing the flow through the center vertical The inlet and outlet of the hole and the eccentric vertical hole are mixed and leaked through the installation seam of the two pieces.

Static seal (19) is also a flat garden cylinder above dynamic seal, and outer diameter and thickness are slightly larger than dynamic seal, and material is softer than dynamic seal, and the contact surface of the two needs finish machining. There is a transverse hole (18, 32) on both sides of the static seal, and its orifice is connected with the liquid inlet and outlet nozzles (17, 33) respectively, and the other end is connected with the central vertical hole (16) and the eccentric vertical hole (34) respectively. ] connected, and the eccentricity of the eccentric vertical hole is the same as the corresponding eccentricity of the dynamic seal. The lower end surface of the static seal has an annular groove (15) with the central vertical hole as the center and the eccentricity of the eccentric vertical hole as the radius. The eccentric vertical hole that annular groove (15) connects two, can form liquid channel.

Compression force mechanism comprises support sleeve (20), elastic body (22), adjustment assembly, installation sleeve (28) and curved arm (27) etc., and adjustment assembly comprises adjustment screw (23) and mounting piece (24). Support sleeve (20) inside, divides upper and lower two parts, and lower part is a short garden cylinder, has a blind hole inlaid static seal (19) at its lower end face. The top of support sleeve (20) is a sleeve, and elastomer (22) and adjustment screw (23) are installed in the inside. Elastomer (22) is the assembly of elastic suitable spring or spring and rubber. Adjusting screw lower end diameter is big, so that press down elastic body (22). The adjusting screw moves up and down in the support sleeve to change the force of the elastic body. Support sleeve adopts moving fit in installation sleeve (28), realizes moving up and down with key and keyway, and does not rotate. The top of the installation sleeve (28) connects a curved arm (27), so that it is inserted in the cover (7), so as to prevent the installation sleeve from rotating when the rotor rotates. Mounting sleeve (28) lower end outer edge processes protruding ring or adorns spring clip and is used for installing ball bearing (31), opens an annular groove or car thread and is used to install the pressing part of bearing inner ring at a certain height from protruding ring. Have the inlet and outlet pipe (25,26) of static seal that straight groove is installed in installing sleeve (28) or support sleeve (20) outer garden cylindrical surface and protruding ring both sides. The adjusting screw is screwed into the center of the mounting piece (24). Mounting part (24) can be made of rubber, and diameter is greater than the about 0.2～0.6 millimeter of mounting sleeve inner diameter, and its mounting position in mounting sleeve changes up and down easily, but because rubber elasticity, stand still on a certain position. Turn the adjustment screw (23) to change the elastic force of the elastomer (22), and adjust the vertical pressure on the contact surface of the dynamic seal (12) and the static seal (19).

Ball bearing unit comprises ball bearing (31), nut (21) and compression piece, and compression piece comprises compression ring (30) and spring clip (29) or compression nut. Ball bearing (31) inner ring is installed on the mounting sleeve (28) lower end outer edge protruding ring or on the spring clip, pushes down with pressure ring (30), locates with spring clip (29) or compresses with compression nut. Ball bearing (31) outer ring is contained on the protruding ring or the spring clip on the inner garden cylindrical surface of rotor pistil body (8) upper section, compresses with nut (21).

Cover (7) has a through hole in the center on the centrifuge chamber (6), and its diameter is slightly larger than the installation sleeve (28), so as to avoid bumping into each other when the rotor rotates. Also have an eccentric hole to be used for inserting the bent arm (27) that is fixed on the mounting sleeve (28) on the cover. The cover is generally made of transparent material (such as plexiglass) to facilitate observation of the rotor. Cover thickness can be selected within 8 ~ 20 mm.

The solution containing the substance to be separated needs to go through the following process in this chromatograph: the solution containing the substance to be separated that is punched in from a liquid supply pump enters the liquid inlet nozzle (17) of the static seal (19) from the liquid inlet pipe (25) , enter the central vertical hole (16) of the static seal along the transverse hole (18), and then go down to the central vertical hole (12) of the dynamic seal (12) and the central vertical hole (9) of the rotor core body (8) and the transverse hole [ 10), the liquid outlet pipe (14) to the spiral capillary (4) on the turntable (5), after a few laps around the rotor, enters the liquid inlet pipe (35) in the rotor core body (8), and passes through the liquid inlet nozzle (36) , horizontal hole (37), eccentric vertical hole (39), upward through the statically sealed eccentric vertical hole (34), diameter horizontal hole (32) and liquid outlet nozzle (33), discharged from the liquid outlet pipe (26), The substances are chromatographically separated in plastic helical capillaries.

Claims (11)

1, comprise driver [1], the centrifugal counter current chromatography instrument of axle sleeve [2] and centrifugal chamber [6], it is characterized in that it is wound with spiral capillary [4] near also being included in the middle part lateral surface, and have centrifugal chromatography rotor and the end face rotary seal mechanism and the lid [7] of a pair of fluid passage on top, the a pair of fluid passage lower port and the spiral capillary [4] of described centrifugal chromatography rotor advance, liquid outlet links to each other, end face rotary seal mechanism comprises motive seal [12] and the static seal [19] that respectively has a pair of fluid passage, snap-in force mechanism and ball bearing unit, motive seal is installed on the top of centrifugal chromatography rotor, static seal is installed on snap-in force mechanism bottom, the static seal another side simultaneously contacts with motive seal and forms the fastness face, on the motive seal fluid passage, lower port links to each other with centrifugal chromatography rotor fluid passage with static seal respectively, ball bearing unit connects centrifugal chromatography rotor and snap-in force mechanism, and lid connects snap-in force mechanism.

2, according to claim 1 described chromatograph, it is characterized in that described centrifugal chromatography rotor comprises rotor block (3), rotating disk (5) and rotor stamen body (8), they all are Cylinder or cone, the rotor block hypomere is connected transferring power with axle sleeve (2), epimere is connected with rotating disk, is wound with spiral capillary (4) near the rotating disk lateral surface, and its internal diameter is 0.2～5 millimeter, disk diameter is 150～450 millimeters, and rotor stamen body is installed on the rotor block center upper portion.

3, chromatograph according to claim 2, it is characterized in that described rotor stamen body (8) is a Cylinder, its center upper portion has a big and mouth blind hole up, garden shape concave surface is arranged at the bottom, hole, one central vertical hole (9) and eccentric upright opening (39) are arranged on concave surface, two holes link to each other separately with two transverse holes (10,37) of rotor stamen body bottom solid part, and lateral aperture is connected with inlet and outlet nozzle of liquid (36,13) respectively; Having on the concave surface with the central vertical hole is that the eccentric throw of center, eccentric upright opening is a ring groove (40) of radius, and groove width is identical with the aperture; One prominent ring or ring groove arranged on the rotor stamen body epimere inner edge, and the outer rim screw thread of having got on the bus.

4, chromatograph according to claim 1, it is characterized in that described motive seal (12) is a flat Cylinder, be embedded on the garden shape concave surface of rotor stamen body (8), have central vertical hole and eccentric upright opening, the upper and lower port in central vertical hole joins with the central vertical hole of static seal and rotor stamen body respectively, and the upper and lower port of eccentric upright opening joins with the ring groove of static seal and rotor stamen body respectively.

5, chromatograph according to claim 1, it is characterized in that described static seal (19) is flat Cylinder, respectively there is a transverse holes relative both sides in outer rim, the aperture links to each other with liquid inlet and outlet mouth (17,33) respectively, the other end in two holes links to each other with eccentric upright opening (34) with central vertical hole (16) respectively, having with the central vertical hole on the lower surface is the center, and the eccentric throw of eccentric upright opening is a ring groove (15) of radius.

6, chromatograph according to claim 1 is characterized in that central vertical hole and the ring groove between described motive seal and the rotor stamen body respectively has an O-ring seal (11,38) on every side.

7, chromatograph according to claim 1, it is characterized in that described snap-in force mechanism comprises supporting sleeve (20), installing sleeve (28), curved boom (27), elastic body (22) and adjusting part, adjusting part comprises adjusting screw (23) and fabricated section (24), supporting sleeve (20) inside is separated into two parts up and down, elastic body (22) and adjusting screw (23) are installed at an upper portion thereof, in the blind hole of lower surface, its underpart, inlay static seal; Supporting sleeve (20) and fabricated section (24) are housed in the installing sleeve (28), and supporting sleeve (20) and installing sleeve (28) adopt has key and keyway movingly and respectively.

8, chromatograph according to claim 7, it is characterized in that described installing sleeve (28), connect curved boom (27) at an upper portion thereof, and the lower end outer rim there is a prominent ring, on prominent ring top one ring groove is arranged, there is straight trough cylinder relative both sides in garden outside installing sleeve and prominent the ring.

9, chromatograph according to claim 7 is characterized in that described fabricated section (24) is a rubber stopper, inserts described adjusting screw (23) at fabricated section (24) center, and its lower end diameter is big, with supporting sleeve (20) internal diameter movingly.

10, chromatograph according to claim 1 is characterized in that described ball bearing unit comprises ball bearing (31), nut (21), pressure ring (30) and Spring Card (29); Ball bearing (31) inner ring is assemblied on the prominent ring of installing sleeve (28) lower end outer rim, pushes down with pressure ring (30), and Spring Card (29) is stuck in the groove on installing sleeve (28) outer rim and locatees.Ball bearing (31) outer ring is loaded on the prominent ring on rotor stamen body (8) the epimere inner edge, and nut (21) cooperates with rotor stamen body (8) epimere.

11, chromatograph according to claim 1 is characterized in that described lid made by the transparent plexiglass plate of 8～20 millimeters thick, and there is a through hole greater than installing sleeve (28) upper diameter in its central authorities, insert the eccentric orfice of curved boom (27) in addition.

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