A pipeline combined single-rotation intelligent countercurrent chromatograph

Abstract

The invention discloses a pipeline-assembled single-rotation intelligent countercurrent chromatograph, which relates to the technical field of countercurrent chromatographs, and comprises a rotating disk, wherein a surrounding separation channel is provided in the rotating disk, wherein a filling block is installed in the surrounding separation channel, wherein one end of the rotating disk is rotatably installed through a liquid slip ring, and the other end of the rotating disk is connected to a main shaft, wherein the main shaft is connected to a driving device, and unwinding is performed by means of a liquid slip ring, so that the rotating disk can complete the unwinding action under single rotation and can rely on the filling block to strengthen the mixing of two phases in the separation channel, thereby abandoning the setting of a planetary gear system, and the main shaft directly drives the main shaft to rotate through the driving device, and the main shaft drives the rotating disk to rotate to realize two-phase separation and extraction, thereby being able to obtain a higher rotation speed and improving the efficiency and effect of separation; secondly, after abandoning the planetary gear system, the equipment noise is greatly reduced, and the device has good dynamic balance.

Description

Technical Field

[0001] The invention relates to the technical field of countercurrent chromatographs, in particular to a pipeline-assembled single-rotation intelligent countercurrent chromatograph. Background Art

[0002] Countercurrent chromatography is a continuous and efficient liquid-liquid distribution chromatography separation technology developed in the 1970s. It generates a two-dimensional force field through synchronous planetary motion of simultaneous revolution and rotation, retains one of the two phases as the stationary phase, and realizes separation and extraction during high-speed rotation. The existing chromatograph needs to unwind the pipeline, so a planetary gear system is used as power transmission, and the pipeline unwinding is realized by the cooperation of revolution and rotation. For specific reference, a cantilever countercurrent chromatograph without a adapter is disclosed in the invention patent, patent number: 2021110888353, but the use of a planetary gear system as power transmission has high noise, low speed, poor dynamic balance, and the speed of the separation column cannot be increased, resulting in poor separation and extraction effect and low efficiency; secondly, the separation column is currently an integrated structure, and the shape of the pipeline cross section is not easy to modify. There is also a 3D printing technology for the production of the separation column. Although the pipeline cross section can be modified, it is impossible to select a suitable manufacturing material, which has great limitations; finally, due to the freedom of revolution and rotation, it is difficult to arrange sensors to realize dynamic monitoring of two-phase separation in traditional chromatographs. Summary of the invention

[0003] The purpose of the present invention is to overcome the deficiencies of the prior art and to provide a pipeline-assembled single-rotation intelligent countercurrent chromatograph to solve the deficiencies of the prior art.

[0004] The objective of the present invention is achieved through the following technical solution: a pipeline-combined single-rotation intelligent countercurrent chromatograph, comprising a rotating disk, a circular separation channel is opened in the rotating disk, one end of the rotating disk is rotatably installed through a liquid slip ring, and the other end of the rotating disk is connected to a main shaft, and the main shaft is connected to a driving device.

[0005] Furthermore, the rotating disk adopts a split structure, including a first rotating disk and a second rotating disk, the first rotating disk is provided with a plurality of threaded holes, the first rotating disk is coaxially connected to the second rotating disk by screws, the first rotating disk and the second rotating disk are provided with half-type separation channels on the opposite end faces, the two groups of the half-type separation channels form the surrounding separation channel, and the first rotating disk is provided with a sealing gasket around the half-type separation channel.

[0006] Furthermore, it also includes a device base plate and a liquid slip ring mounting seat, the liquid slip ring mounting seat is arranged on the device base plate, the liquid slip ring includes a rotary joint and a liquid slip ring mounting shaft, one end of the rotary joint is installed on the liquid slip ring mounting seat, and the other end is rotatably connected to the liquid slip ring mounting shaft, and the liquid slip ring mounting shaft is connected to the first rotating disk.

[0007] Furthermore, a plurality of filling blocks are connected in the circular separation channel by screws, and the plurality of filling blocks are evenly distributed along the trajectory path of the circular separation channel.

[0008] Furthermore, the rotating disk is provided with a plurality of detection holes, which are arranged at intervals along the radial direction of the rotating disk, the detection holes are connected to the annular separation channel, the rotating disk is provided with a sensor at the position of each detection hole, and the detection axis of the sensor is arranged in the annular separation channel through the detection hole.

[0009] Furthermore, the sensor is one or more of a pressure sensor, an acceleration sensor, and a concentration sensor.

[0010] Furthermore, a first vertical plate is fixed on the bottom plate of the equipment, a first bearing seat is arranged on the first vertical plate, the first bearing seat is mounted on the main shaft, an electric slip ring is mounted on the main shaft, and the sensor is wired through the electric slip ring.

[0011] Furthermore, a second vertical plate is fixed on the base plate of the equipment, the second vertical plate and the first vertical plate are spaced apart along the axial direction of the main shaft, a second bearing seat is installed on the second vertical plate, the second bearing seat is mounted on the main shaft, the driving device includes a driving motor and a synchronous belt, the driving motor is installed on the base plate of the equipment, the output shaft of the driving motor is mounted with a first synchronous pulley, the main shaft is mounted with a second synchronous pulley, and the second synchronous pulley is connected to the first synchronous pulley through the synchronous belt transmission.

[0012] Furthermore, an encoder bracket is fixed on the second vertical plate, and an encoder is installed on the encoder bracket.

[0013] Furthermore, the rotating disk is provided with a separation column end inlet and a separation column end outlet, the separation column end inlet and the separation column end outlet are respectively connected to the two ends of the surrounding separation channel, and the liquid slip ring is provided with a rotary joint end inlet and a rotary joint end outlet.

[0014] The beneficial effects of the present invention are:

[0015] 1. The present invention adopts a liquid slip ring to perform unwinding, so that the rotating disk can complete the unwinding action under single rotation, thereby abandoning the setting of the planetary gear system, directly driving the main shaft to rotate through the driving device, and the main shaft drives the rotating disk to rotate to realize two-phase separation and extraction, which can obtain a higher rotation speed and improve the separation efficiency and effect; secondly, after abandoning the planetary gear system, the equipment noise is greatly reduced, and it has better dynamic balance.

[0016] 2. Under the arrangement of single rotation, the rotating disk can be set to a split type. After the rotating disk is disassembled, the half-type separation channels on the first rotating disk and the second rotating disk are open, and the half-type separation channels of any shape can be processed by CNC machine tools respectively, and the range of selectable materials is wide, so that the surrounding separation channel formed by the two half-type separation channels can be modified to meet different needs.

[0017] 3. Since the rotating disk has only rotational freedom, the sensor can be unwound through the electric slip ring, so that the sensor can be arranged on the rotating disk to realize dynamic monitoring of the sample concentration, liquid flow rate and other states of the sample separation process. It can also detect the sealing of the circular separation channel to prevent leakage, making the countercurrent chromatograph safer and smarter.

[0018] 4. Since the rotating disk adopts a split structure, after the first rotating disk and the second rotating disk are disassembled, it is convenient to process and install the filling blocks independently. By installing filling blocks of different shapes in the surrounding separation channel, the cross-sectional shape of the flow channel can be changed, thereby realizing the regulation of the disturbance amount of the two-phase mixing interface in the flow channel. This is conducive to accelerating the movement state of the sample at the two-phase interface, improving the distribution coefficient difference between the two phases, improving the separation efficiency, and solving the problem of low separation efficiency in the single rotation mode. BRIEF DESCRIPTION OF THE DRAWINGS

[0019] Figure 1 A three-dimensional schematic diagram of a pipeline combined single self-rotating intelligent countercurrent chromatograph of the present invention Figure 1 ;

[0020] Figure 2 A three-dimensional schematic diagram of a pipeline combined single self-rotating intelligent countercurrent chromatograph of the present invention Figure 2 ;

[0021] Figure 3 It is a schematic structural diagram of the second rotating disk in a pipeline-assembled single-rotating intelligent countercurrent chromatograph of the present invention;

[0022] Figure 4 It is a structural schematic diagram of the first rotating disk in a pipeline-assembled single-rotating intelligent countercurrent chromatograph of the present invention;

[0023] In the figure, 1-rotating disk, 2-surrounding separation channel, 3-liquid slip ring, 4-main shaft, 5-first rotating disk, 6-second rotating disk, 7-equipment bottom plate, 8-liquid slip ring mounting seat, 9-rotating joint, 10-liquid slip ring mounting shaft, 11-filling block, 12-detection hole, 13-sensor, 14-first vertical plate, 15-first bearing seat, 16-electric slip ring, 17-second vertical plate, 18-second bearing seat, 19-driving motor, 20-synchronous belt, 21-first synchronous pulley, 22-second synchronous pulley, 23-encoder bracket, 24-encoder, 25-separation column end inlet, 26-separation column end outlet, 27-rotating joint end inlet, 28-rotating joint end outlet, 29-threaded hole, 30-sealing gasket. DETAILED DESCRIPTION

[0024] The technical solution of the present invention is further described in detail below in conjunction with the accompanying drawings, but the protection scope of the present invention is not limited to the following.

[0025] Embodiment 1

[0026] Traditional chromatographs need to use planetary gear trains to complete the unwinding action. However, the planetary gear trains have disadvantages such as low speed, high noise, and poor dynamic balance, which result in that the separation efficiency and separation effect of the countercurrent chromatograph cannot be effectively improved, limiting the development of the countercurrent chromatograph. To this end, the present application provides a new design idea, specifically:

[0027] like Figures 1 to 4 As shown, a pipeline combined single self-rotating intelligent countercurrent chromatograph comprises a rotating disk 1, a surrounding separation channel 2 is provided in the rotating disk 1, one end of the rotating disk 1 is rotatably installed through a liquid slip ring 3, the other end of the rotating disk 1 is connected to a main shaft 4, the main shaft 4 is connected to a driving device, a solvent pipeline is installed through the liquid slip ring 3, the solvent pipeline is connected to the rotating disk 1, so that the solvent is passed into the surrounding separation channel 2, under the action of the liquid slip ring 3, the solvent pipeline follows the rotating disk 1 and the liquid slip ring 3 to rotate together, so that the solvent pipeline is unwound, so that the rotating disk 1 only needs to be provided with a rotating The degree of freedom can realize the separation operation and complete the unwinding, so that the setting of the planetary gear system can be abandoned, the equipment investment cost of the chromatograph is reduced, the structure is more compact, and the main shaft 4 is directly driven by the driving device to rotate, and the main shaft 4 drives the rotating disk 1 to rotate to realize the two-phase separation and extraction. Since there is no deceleration effect of the planetary gear system, the main shaft 4 can obtain a higher rotation speed, and a higher distribution coefficient difference is quickly obtained from the surrounding separation channel 2, thereby improving the separation efficiency and effect; secondly, after abandoning the planetary gear system, the equipment noise is greatly reduced, and it has better dynamic balance.

[0028] Embodiment 2

[0029] The extraction channel inside the traditional separation column is generally set as a single channel, and it is impossible to set a complex extraction channel. The complex extraction channel can only be processed by 3D printing, but the material cannot be selected. Therefore, based on the first embodiment, as shown in FIG. Figure 1 , Figure 3 and Figure 4 As shown, the rotating disk 1 adopts a split structure, including a first rotating disk 5 and a second rotating disk 6. The first rotating disk 5 is provided with a plurality of threaded holes 29. The first rotating disk 5 is coaxially connected with the second rotating disk 6 by screws. The opposite end surfaces of the first rotating disk 5 and the second rotating disk 6 are provided with half-type separation channels. The two groups of half-type separation channels form a surrounding separation channel 2. The first rotating disk 5 is provided with a sealing gasket 30 around the half-type separation channel to improve the sealing performance between the first rotating disk 5 and the second rotating disk 6. The rotating disk 1 is split into the first rotating disk 5 and the second rotating disk 6. A half-type separation channel is milled on the end face of the second rotating disk 6, and a half-type separation channel is milled on the end face of the second rotating disk 6 near the first rotating disk 5. The two half-type separation channels are symmetrically arranged along the radial plane of the rotating disk 1, so that after the first rotating disk 5 and the second rotating disk 6 are connected together, the two half-type separation channels can form a surrounding separation channel 2. By adjusting the milling path, a variety of surrounding separation channels 2 of different shapes can be processed, so that the surrounding separation channel 2 can be modified to meet different needs. At the same time, the influence of surrounding separation channels 2 of different shapes on separation effect and separation efficiency can also be studied.

[0030] Embodiment 3

[0031] Based on the second embodiment, Figure 1 and Figure 2As shown, it also includes an equipment base plate 7 and a liquid slip ring mounting seat 8, the liquid slip ring mounting seat 8 is arranged on the equipment base plate 7, the liquid slip ring 3 includes a rotary joint 9 and a liquid slip ring mounting shaft 10, one end of the rotary joint 9 is mounted on the liquid slip ring mounting seat 8, and the other end is rotatably connected to the liquid slip ring mounting shaft 10, the liquid slip ring mounting shaft 10 is connected to the first rotating disk 5, and a separation column end inlet 25 and a separation column end outlet 26 are arranged on the rotating disk 1, and the separation column end inlet 25 and the separation column end outlet 26 are respectively connected to the two ends of the surrounding separation channel 2, and a rotary joint end inlet 27 and a rotary joint end outlet 28 are arranged on the liquid slip ring 3. Preferably, the rotary joint end inlet 27 and the rotary joint end outlet 28 are arranged on the rotary joint. 9, the rotary joint 9 is fixedly mounted on the liquid slip ring mounting seat 8, and there is relative rotational freedom between the rotary joint 9 and the liquid slip ring mounting shaft 10. The separation column end inlet 25 is connected to the liquid inlet port of the liquid slip ring mounting shaft 10 through the liquid inlet pipe, and the separation column end outlet 26 is connected to the liquid outlet port of the liquid slip ring mounting shaft 10 through the liquid outlet pipe. The solvent enters the surrounding separation channel 2 through the rotary joint end inlet 27, the liquid slip ring mounting shaft 10 and the liquid inlet pipe. During the rotation of the rotating disk 1, the liquid slip ring mounting shaft 10 rotates together, so that the liquid inlet pipe and the liquid outlet pipe on it rotate together to achieve unwinding, and the separated liquid is discharged through the liquid outlet pipe, the liquid slip ring mounting shaft 10 and the rotary joint end outlet 28.

[0032] Embodiment 4

[0033] Based on the third embodiment, Figure 1 and Figure 2 As shown, a first vertical plate 14 is fixed on the equipment bottom plate 7, a first bearing seat 15 is arranged on the first vertical plate 14, and the first bearing seat 15 is sleeved on the main shaft 4, a second vertical plate 17 is fixed on the equipment bottom plate 7, the second vertical plate 17 and the first vertical plate 14 are spaced apart along the axial direction of the main shaft 4, a second bearing seat 18 is installed on the second vertical plate 17, and the second bearing seat 18 is sleeved on the main shaft 4, the driving device includes a driving motor 19 and a synchronous belt 20, the driving motor 19 is installed on the equipment bottom plate 7, the output shaft of the driving motor 19 is sleeved with a first synchronous pulley 21, and the main shaft 4 is provided with a first vertical plate 17. A second synchronous pulley 22 is mounted on the shaft 4, and the second synchronous pulley 22 is connected to the first synchronous pulley 21 through a synchronous belt 20. The driving motor 19 drives the first synchronous pulley 21 to rotate, and the first synchronous pulley 21 drives the second synchronous pulley 22 to rotate through the synchronous belt 20. The second synchronous pulley 22 drives the main shaft 4 to rotate, and the main shaft 4 drives the rotating disk 1 to rotate for extraction and separation. The driving motor 19 can provide a high speed, and the rotating disk 1 can obtain a high speed without a planetary gear system to reduce speed, thereby improving the separation efficiency. The structure is stable and the dynamic balance is good.

[0034] Embodiment 5

[0035] In addition to realizing pipeline unwinding, the traditional chromatograph adopts a planetary gear system, and also needs to make the separation column generate an eccentric centripetal force under the action of rotation and revolution, thereby accelerating the separation. After abandoning the setting of the planetary gear system, it is necessary to solve the problem of low solvent movement intensity in the single rotation mode. For this purpose, based on the fourth embodiment, as shown in FIG. Figures 1 to 3 As shown, a plurality of filling blocks 11 are connected by screws in the annular separation channel 2, and the plurality of filling blocks 11 are evenly distributed along the trajectory path of the annular separation channel 2. When the rotating disk 1 rotates at a high speed, the solvent in the annular separation channel 2 will frequently collide with the filling blocks 11 in the process of moving toward the separation column end outlet 26, so that the solvent moves irregularly, the movement intensity is enhanced, and a higher distribution coefficient difference can be quickly achieved, thereby improving the separation efficiency; secondly, the split structure of the rotating disk 1 facilitates the installation of the filling blocks 11, and the arrangement position can also be adjusted arbitrarily. After the first rotating disk 5 and the second rotating disk 6 are separated, the filling blocks 11 are installed in the annular separation channel 2 with screws, and the disassembly and assembly are simple and quick; in specific implementation, a plurality of threaded holes are opened in the semi-type separation channel along its own trajectory direction at equal intervals for installing the filling blocks 11.

[0036] Embodiment 6

[0037] Since the conventional separation column has both rotation and revolution degrees of freedom, it is very difficult to wire the detection device. Therefore, the conventional chromatograph does not have an online detection function and cannot understand the separation state in real time. Therefore, based on the fifth embodiment, as shown in FIG. Figure 1 and Figure 2As shown, a plurality of detection holes 12 are provided on the rotating disk 1, and the plurality of detection holes 12 are arranged at intervals along the radial direction of the rotating disk 1, and the detection holes 12 are connected to the encircling separation channel 2. A sensor 13 is installed at the position of each detection hole 12 of the rotating disk 1, and the detection axis of the sensor 13 is arranged in the encircling separation channel 2 through the detection hole 12. An electric slip ring 16 is mounted on the main shaft 4, and the sensor 13 is wired through the electric slip ring 16. After the chromatograph is changed to a single rotation, it is only necessary to overcome the winding problem caused by the rotation. The electric slip ring 16 is mounted on the main shaft 4, and the wire of the sensor 13 is wired through the electric slip ring 16, so that the unwinding of the wire of the sensor 13 is realized, so that the sensor 13 can be arranged on the rotating disk 1 to dynamically monitor the separation process. Preferably, the sensor 13 is one or more of a pressure sensor, an acceleration sensor, and a concentration sensor, and the sensor 13 is arranged in a plurality of groups. , each group of monitored data is different, and each group includes multiple identical sensors. Multiple sensors 13 are arranged in sequence along the path of the circular separation channel 2, so that the dynamic changes of the separation process can be obtained, and dynamic monitoring of the separation can be realized. Specifically, one group of sensors uses a pressure sensor to detect the pressure value of each section on the circular separation channel 2, and implements monitoring of the sealing performance in the rotating disk 1 to prevent leakage, thereby improving the safety of use; one group of sensors uses a concentration sensor to detect the solvent concentration of each section on the circular separation channel 2, so as to obtain the separation situation of the solvent, thereby judging the separation efficiency; one group of sensors uses an acceleration sensor to detect the flow rate of the solvent, and judges the impact on the movement of the solvent at different rotation speeds. In summary, real-time dynamic monitoring of the separation process is realized through different sensors, and each performance state in the separation process is obtained, which is convenient for timely adjustment and makes the chromatograph intelligent.

[0038] Furthermore, an encoder bracket 23 is fixed on the second vertical plate 17 , and an encoder 24 is installed on the encoder bracket 23 . The encoder 24 is used to monitor the displacement of the main shaft 4 in real time, thereby improving the dynamic balance of the chromatograph.

Claims

1. A pipeline combined single-rotation intelligent countercurrent chromatograph, characterized in that: The invention comprises a rotating disk (1), wherein a surrounding separation channel (2) is provided in the rotating disk (1), one end of the rotating disk (1) is rotatably mounted via a liquid slip ring (3), the liquid slip ring (3) being used to mount a solvent pipeline, the solvent pipeline being connected to the rotating disk (1) so that the solvent pipeline rotates along with the rotating disk (1) and the liquid slip ring (3), the other end of the rotating disk (1) being connected to a main shaft (4), and the main shaft (4) being connected to a driving device; The rotating disk (1) adopts a split structure, comprising a first rotating disk (5) and a second rotating disk (6), the first rotating disk (5) being provided with a plurality of threaded holes (29), the first rotating disk (5) being coaxially connected to the second rotating disk (6) by means of screws, the first rotating disk (5) and the second rotating disk (6) being provided with half-shaped separation channels on opposite end surfaces, the two groups of the half-shaped separation channels forming the surrounding separation channel (2), the first rotating disk (5) being provided with a sealing gasket (30) around the half-shaped separation channel; A plurality of filling blocks (11) are connected in the encircling separation channel (2) by means of screws, and the plurality of filling blocks (11) are evenly distributed along the trajectory path of the encircling separation channel (2); The rotating disk (1) is provided with a plurality of detection holes (12), the plurality of detection holes (12) being arranged at intervals along the radial direction of the rotating disk (1), the detection holes (12) being connected to the encircling separation channel (2), the rotating disk (1) being provided with a sensor (13) at the position of each detection hole (12), the detection axis of the sensor (13) being arranged in the encircling separation channel (2) through the detection hole (12).

2. The pipeline combined single-rotation intelligent countercurrent chromatograph according to claim 1, characterized in that: It also comprises an equipment base plate (7) and a liquid slip ring mounting seat (8), wherein the liquid slip ring mounting seat (8) is arranged on the equipment base plate (7), and the liquid slip ring (3) comprises a rotary joint (9) and a liquid slip ring mounting shaft (10), wherein one end of the rotary joint (9) is mounted on the liquid slip ring mounting seat (8), and the other end is rotatably connected to the liquid slip ring mounting shaft (10), and the liquid slip ring mounting shaft (10) is connected to the first rotating disk (5).

3. The pipeline combined single-rotation intelligent countercurrent chromatograph according to claim 2 is characterized in that: The sensor (13) is one or more of a pressure sensor, an acceleration sensor, and a concentration sensor.

4. The pipeline combined single-rotation intelligent countercurrent chromatograph according to claim 2, characterized in that: A first vertical plate (14) is fixed on the equipment bottom plate (7), a first bearing seat (15) is arranged on the first vertical plate (14), the first bearing seat (15) is sleeved on the main shaft (4), an electric slip ring (16) is sleeved on the main shaft (4), and the sensor (13) is wired via the electric slip ring (16).

5. The pipeline combined single-rotation intelligent countercurrent chromatograph according to claim 4, characterized in that: A second vertical plate (17) is fixed on the equipment base plate (7), the second vertical plate (17) and the first vertical plate (14) are spaced apart along the axial direction of the main shaft (4), a second bearing seat (18) is mounted on the second vertical plate (17), and the second bearing seat (18) is sleeved on the main shaft (4), the driving device comprises a driving motor (19) and a synchronous belt (20), the driving motor (19) is mounted on the equipment base plate (7), the output shaft of the driving motor (19) is sleeved with a first synchronous belt pulley (21), the main shaft (4) is sleeved with a second synchronous belt pulley (22), and the second synchronous belt pulley (22) is connected to the first synchronous belt pulley (21) through the synchronous belt (20).

6. The pipeline combined single-rotation intelligent countercurrent chromatograph according to claim 5, characterized in that: An encoder bracket (23) is fixed on the second vertical plate (17), and an encoder (24) is mounted on the encoder bracket (23).

7. The pipeline combined single-rotation intelligent countercurrent chromatograph according to claim 1, characterized in that: The rotating disk (1) is provided with a separation column end inlet (25) and a separation column end outlet (26), the separation column end inlet (25) and the separation column end outlet (26) are respectively connected to the two ends of the surrounding separation channel (2), and the liquid slip ring (3) is provided with a rotary joint end inlet (27) and a rotary joint end outlet (28).

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