A single spin counter-current chromatography high mass transfer separation column

Abstract

The application relates to the technical field of countercurrent chromatography, in particular to a high-mass-transfer separation column of a single-rotation countercurrent chromatograph, which comprises a separation column bottom plate installed on a main shaft, a power amplification plate hung on the separation column bottom plate and connected with an ultrasonic wave generator, a spiral groove being arranged on the power amplification plate, a spiral tube embedded in the spiral groove, a spiral tube pressing plate arranged above the spiral tube, a separation column top plate arranged above the spiral tube pressing plate, and an adapter assembly arranged on the separation column top plate and used for connecting an external feeding pipe with an inlet and an outlet of the spiral tube. The planar coil pipe structure formed by winding a single continuous pipe is adopted to replace the traditional split type combined structure, so that the sealing leakage risk of the combined surface is eliminated; the interphase mass transfer is realized by the ultrasonic wave generator to realize online dynamic regulation and control, so that the separation efficiency is obviously improved; the modular design simplifies the manufacturing process, and the cost and maintenance difficulty are reduced.

Description

Technical Field

[0001] This invention relates to the field of countercurrent chromatography technology, and more particularly to a high mass transfer separation column for a single-rotation countercurrent chromatograph. Background Technology

[0002] Countercurrent chromatography is a continuous and efficient liquid-liquid partition chromatography method that utilizes the relative motion of two solvent phases within a separation column to achieve sample separation and purification. As the core component of a countercurrent chromatograph, the structural design of the separation column directly affects the separation efficiency.

[0003] Traditional countercurrent chromatography columns often employ a synchronous planetary self-unwinding structure, using a planetary gear mechanism to achieve the column's revolution and rotation to maintain fluid balance. However, this structure suffers from problems such as complex mechanism, high manufacturing cost, and difficult maintenance. To address these shortcomings, single-rotation separation columns based on rotary joints have been developed in recent years. Chinese invention patent CN119438462B discloses a pipeline-combined single-rotation intelligent countercurrent chromatograph that uses a liquid slip ring for unwinding, allowing the rotating disk to complete the unwinding action under single rotation, abandoning the traditional planetary gear system, increasing rotational speed, and reducing noise. This patent features a ring-shaped separation channel within the rotating disk, with multiple packing blocks evenly distributed along the trajectory path within the channel. The physical collision of the packing blocks with the flowing solvent disturbs the two-phase interface, enhancing interphase mixing and mass transfer.

[0004] However, existing single-rotation countercurrent chromatography separation columns still have the following technical defects: (1) Limited mass transfer efficiency; the physical disturbance of the packing blocks is used to enhance interphase mixing, and its effect depends on the flow state of the fluid between the packing blocks. For high-viscosity samples or substances with low diffusion coefficients, the disturbance intensity of the packing blocks on the interface between the two phases is insufficient, and the mass transfer effect of the sample between the two phases is difficult to be fully activated, thus limiting the separation efficiency. In addition, the structure of the packing blocks is fixed, and the disturbance intensity cannot be adjusted during equipment operation, making it difficult to adapt to the separation requirements of different samples. (2) Insufficient sealing reliability; single-rotation separation columns mostly adopt a split structure, with the rotating disk composed of a first rotating disk and a second rotating disk. The opposite end faces of the two are opened with semi-shaped separation channels, and the combined surface needs to be sealed with a sealing gasket. Under long-term operation or high-pressure conditions, the sealing ring is prone to aging, wear, or improper installation, leading to solvent leakage and affecting the stability and safety of the system. At the same time, the split structure requires high processing precision, increasing manufacturing costs. (3) Complex manufacturing process; the ring-shaped separation channel of the single self-rotating separation column needs to be formed by milling on a rotary table by a CNC machine tool. It is difficult to process complex flow channel shapes, the material selection is limited, and it is difficult to flexibly modify the flow channel cross-section. Although the split structure is easy to process, it still requires high-precision matching, which increases the manufacturing difficulty and cost. (4) Insufficient adjustment flexibility; the filling block is fixed and cannot be adjusted in position or shape during equipment operation. For samples with different properties, it is difficult to optimize the mixing intensity and separation conditions in real time, which limits the applicability of the instrument and further improvement of the separation effect. Summary of the Invention

[0005] The purpose of this invention is to provide a high mass transfer separation column for a single-rotation countercurrent chromatograph. While maintaining the advantages of the single-rotation structure, this separation column further improves the mass transfer efficiency, sealing reliability, manufacturing convenience, and control flexibility.

[0006] To achieve the above objectives, the present invention adopts the following technical solution:

[0007] A high-mass-transfer separation column for a single-rotation countercurrent chromatograph includes an ultrasonic generator, a column base plate, a power amplifier plate, a spiral tube, a spiral tube clamping plate, and a column top plate.

[0008] The separation column base plate is mounted on the main shaft of the countercurrent chromatograph and rotates synchronously with the main shaft; multiple mounting ports are evenly opened on it along the circumferential direction, and a power amplifier board is installed in each mounting port. The power amplifier board is connected to the ultrasonic generator. The power amplifier board does not contact the separation column base plate and can vibrate freely under ultrasonic excitation.

[0009] The bottom surface of the power amplifier board is provided with a spiral groove, and the spiral tube is located in the spiral groove. The spiral tube is a planar coil structure with a central hole formed by winding a single continuous pipe.

[0010] A frustum is provided on the centerline of the bottom plate of the separation column. The spiral tube and the spiral tube pressure plate are sleeved on the frustum. The spiral tube pressure plate is located above the spiral tube and is used to fix the spiral tube.

[0011] The top plate of the separation column is disposed above the spiral tube pressure plate and is used to press the spiral tube pressure plate and the spiral tube together, and is fixedly connected to the bottom plate of the separation column; the inlet end and outlet end of the spiral tube both pass through the top plate of the separation column.

[0012] Furthermore, the ultrasonic generator is connected to the power amplifier board via a double-ended stud; and the ultrasonic generator is fastened to the bottom plate of the separation column by an anti-loosening ring;

[0013] The outer shell of the ultrasonic generator has a conical structure, and the anti-loosening ring has a conical hole that fits into the conical structure.

[0014] Furthermore, the spiral groove shape of the power amplifier board is fitted to the outer diameter of the spiral tube, allowing the spiral tube to be embedded in the spiral groove of the power amplifier board.

[0015] Furthermore, the spiral tube pressure plate is a cross structure with a central hole, and a slot communicating with the central hole is opened on the side away from the spiral tube. A stop ring is provided above the spiral tube pressure plate, and the circumference of the stop ring is provided with protrusions that engage with the slot, so as to achieve circumferential fixation of the stop ring and the spiral tube pressure plate, and realize that the spiral tube pressure plate and the spiral tube rotate synchronously.

[0016] Furthermore, the top plate of the separation column is provided with strip-shaped mounting holes for the inlet and outlet ends of the spiral tube to extend out.

[0017] Furthermore, both the inlet and outlet ends of the spiral tube are connected to a transition assembly;

[0018] The adapter assembly includes an adapter plate, an adapter seat, and an adapter connector; the adapter plate is fixed to the top plate of the separation column, and the adapter seat is provided on it. The adapter seat has a flow channel, and adapter connectors are connected to both ends of the flow channel, which are respectively connected to the inlet or outlet end of the spiral tube and the external feeding pipe.

[0019] Compared with the prior art, the present invention has the following beneficial effects:

[0020] (1) The planar coil structure formed by winding a single continuous pipe has no combined sealing structure. This fundamentally eliminates the risk of leakage caused by seal failure, enabling the separation column to maintain excellent sealing reliability and significantly improving the safety and stability of the instrument. At the same time, the spiral tube formed by winding does not require precision machining, simplifying the manufacturing process and reducing manufacturing costs.

[0021] (2) An ultrasonic-assisted mass transfer technology combining an ultrasonic generator and a power amplifier board is adopted; by vibrating the fluid with ultrasonic waves and disturbing the interface between the two phases, the mass transfer between phases is significantly enhanced, thereby improving the separation efficiency and separation degree. At the same time, the output power and frequency of the ultrasonic waves can be adjusted online during the separation process, and the separation conditions can be optimized according to the sample properties, thus expanding the applicability of the instrument and improving the separation effect.

[0022] (3) The anti-loosening ring’s conical surface fit structure effectively prevents the threaded connection of the ultrasonic generator from loosening under high-speed rotation; the locking ring and the spiral tube pressure plate’s groove fit ensure that the spiral tube pressure plate and the spiral tube rotate synchronously, preventing slippage and wear; it improves the stability and reliability of the instrument in long-term operation and extends the service life of the equipment.

[0023] (4) The modular design allows for independent disassembly and assembly of components such as the power amplifier board, spiral tube, and spiral tube pressure plate. The spiral tube pressure plate design makes the spiral tube installation process simple and quick; the locking ring and the spiral tube pressure plate groove ensure synchronous rotation and facilitate disassembly and maintenance; thus improving the convenience of installation and maintenance and reducing maintenance costs and time. Attached Figure Description

[0024] Figure 1 This is a schematic diagram of the exploded structure of the present invention.

[0025] Figure 2 This is a schematic diagram of the structure of the present invention.

[0026] Figure 3 This is a cross-sectional structural diagram of the present invention.

[0027] Figure 4 This is a schematic diagram of the separation column base plate structure of the present invention.

[0028] Figure 5 This is a schematic diagram of the structure of the spiral tube, spiral tube pressure plate and stop ring of the present invention.

[0029] Figure 6 This is a schematic diagram of the structure of the adapter component of the present invention.

[0030] The markings in the diagram are: 1. Main shaft; 2. Anti-loosening ring; 3. Ultrasonic generator; 4. Double-ended stud; 5. Separator column base plate; 6. Power amplifier board; 7. Spiral tube; 8. Spiral tube pressure plate; 9. Locking ring; 10. Separator column top plate; 11. Adapter plate; 12. Adapter seat; 13. Adapter connector. Detailed Implementation

[0031] The technical solutions of the present invention will be clearly and completely described below with reference to the accompanying drawings of the embodiments of the present invention. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments.

[0032] like Figure 1 , Figure 2 and Figure 3 As shown, this embodiment provides a high mass transfer separation column for a single-rotation countercurrent chromatograph, which is mounted on the main shaft 1 of the countercurrent chromatograph via positioning grooves and screws, and rotates synchronously with the main shaft 1. The separation column includes an ultrasonic generator 3, a column base plate 5, a power amplifier board 6, a spiral tube 7, a spiral tube clamping plate 8, a stop ring 9, a column top plate 10, and an adapter assembly.

[0033] like Figure 4 As shown, the separation column base plate 5 is a disc-shaped structure with a mounting groove for fixing the main shaft 1 on one side of its center, and a frustum coaxial with the main shaft 1 on the other side; the separation column base plate 5 has multiple mounting openings along the circumference, and each mounting opening contains a power amplifier board 6. The power amplifier board 6 does not contact the separation column base plate 5 on all four sides, but is installed in the mounting opening of the separation column base plate 5 through a four-corner suspension structure to achieve the effect of vibration amplification.

[0034] The ultrasonic generator 3 is connected to the power amplifier board 6 via a double-ended stud 4 and is secured to the base plate 5 of the separation column by an anti-loosening ring 2. The anti-loosening ring 2 has a conical hole that fits into the conical shell of the ultrasonic generator 3 to prevent the threaded connection from loosening due to vibration during instrument operation.

[0035] The surface of the power amplifier board 6 is provided with a spiral groove that fits with the outer diameter of the spiral tube 7; the spiral tube 7 is a planar coil structure with a central hole formed by winding a single continuous pipe and is embedded in the spiral groove of the power amplifier board 6, so that the spiral tube 7 fits tightly with the power amplifier board 6, ensuring that the ultrasonic energy is effectively transmitted to the fluid in the spiral tube 7.

[0036] like Figure 5As shown, the spiral tube 7, spiral tube pressure plate 8, and stop ring 9 are fitted onto the truncated cone of the separation column base plate 5. The spiral tube pressure plate 8 is positioned above the spiral tube 7 and is used to install and fix the spiral tube 7. During installation, after installing a section of the spiral tube 7 into the spiral groove of the power amplifier board 6, the spiral tube pressure plate 8 is rotated to press down the installed spiral tube 7, preventing it from falling off during subsequent installation. The spiral tube pressure plate 8 is a cross-shaped structure with a central opening, and its side has a slot communicating with the central opening. Each bracket has a notch at its port for the outlet end of the spiral tube 7 to extend out. The stop ring 9 is positioned above the spiral tube pressure plate 8 and has three protrusions and one notch. The three protrusions cooperate with the slots of the spiral tube pressure plate 8 to achieve circumferential positioning of the stop ring 9 and the spiral tube pressure plate 8, and to achieve a fixed connection between the spiral tube pressure plate 8 and the separation column base plate 5. The notch is used for the inlet end of the spiral tube 7 to extend out. The stop ring 9 ensures that the spiral tube pressure plate 8 and the spiral tube 7 rotate synchronously during the operation of the instrument, and avoids the spiral tube pressure plate 8 slipping on the surface of the spiral tube 7, which would cause wear and abnormal noise.

[0037] The top plate 10 of the separation column is disposed above the spiral tube pressure plate 8 and the stop ring 9, and is fixedly connected to the bottom plate 5 of the separation column, for pressing the spiral tube pressure plate 8 and the spiral tube 7 together. The top plate 10 of the separation column has strip-shaped mounting holes for the inlet and outlet ends of the spiral tube 7 to extend out; the inlet and outlet ends of the spiral tube 7 are both connected to adapter components.

[0038] like Figure 6 As shown, the adapter assembly includes an adapter plate 11, an adapter seat 12, and an adapter 13. The adapter plate 11 is mounted on the top plate 10 of the separation column by screws. The adapter seat 12 is fixed on the adapter plate 11 and has a fluid channel inside. Both ends of the fluid channel are connected to adapters 13 for connecting the outlet end of the external feeding pipe, the inlet end of the external feeding pipe, and the inlet and outlet ends of the spiral pipe 7.

[0039] During operation, the separation column is mounted on a countercurrent chromatograph via a spindle. The countercurrent chromatograph's drive unit rotates the spindle via a synchronous belt, thereby causing the entire separation column to rotate synchronously at high speed. After the separation column reaches the set rotation speed, two immiscible solvents are sequentially pumped into the spiral tube through the inlet end of an external feed tube, flowing through the entire spiral tube and then exiting from the outlet end of the external feed tube. Pumping continues until the two solvent phases establish a stable dynamic equilibrium within the spiral tube under the influence of the rotating centrifugal force field. Once the two phases are in equilibrium, the sample solution is injected into the spiral tube through the inlet end of the external feed tube. All ultrasonic generators are activated, generating ultrasonic waves that are transmitted to the fluid within the spiral tube through a power amplifier board. The ultrasonic waves vibrate the fluid, disturbing the two-phase interface and promoting vigorous interphase mass transfer of the sample as it traverses the two solvent phases, thereby achieving efficient and continuous extraction and separation of the components within the sample.

[0040] During the separation process, the output power and frequency of the ultrasonic generator can be adjusted online according to the sample properties and separation requirements to optimize mass transfer conditions. The separated components flow out with the solvent from the outlet end of the spiral tube, are discharged through the outlet end of the external feed tube, and are collected.

[0041] The above description is only a preferred embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Any equivalent substitutions or modifications made by those skilled in the art within the scope of the technology disclosed in the present invention, based on the technical solution and inventive concept of the present invention, should be covered within the scope of protection of the present invention.

Claims

1. A high-mass-transfer separation column for a single-rotation countercurrent chromatograph, characterized in that, It includes an ultrasonic generator (3), a separation column base plate (5), a power amplifier board (6), a spiral tube (7), a spiral tube pressure plate (8), and a separation column top plate (10). The separation column base plate (5) is mounted on the main shaft (1) of the countercurrent chromatograph and rotates synchronously with the main shaft (1); multiple mounting ports are evenly opened on it along the circumferential direction, and a power amplifier board (6) is provided in each mounting port. The power amplifier board (6) is connected to the ultrasonic generator (3). The power amplifier board (6) does not contact the separation column base plate (5) and can vibrate freely under ultrasonic excitation. The power amplifier board (6) has a spiral groove on the side away from the main shaft (1), and the spiral tube (7) is located in the spiral groove. The spiral tube (7) is a planar coil structure with a central hole formed by winding a single continuous pipe. The bottom plate (5) of the separation column is provided with a frustum on the center line of the side away from the main shaft (1). The spiral tube (7) and the spiral tube pressure plate (8) are sleeved on the frustum. The spiral tube pressure plate (8) is located on the side of the spiral tube (7) away from the main shaft and is used to fix the spiral tube (7). The top plate (10) of the separation column is located on the side of the spiral tube pressure plate (8) away from the main shaft (1) and is used to press the spiral tube pressure plate (8) and the spiral tube (7) together and is fixedly connected to the bottom plate (5) of the separation column; the inlet end and outlet end of the spiral tube (7) both pass through the top plate (10) of the separation column.

2. The high mass transfer separation column for a single-rotation countercurrent chromatograph according to claim 1, characterized in that, The ultrasonic generator (3) is connected to the power amplifier board (6) via a double-headed stud (4); and the ultrasonic generator (3) is fastened to the bottom plate (5) of the separation column by an anti-loosening ring (2); The outer shell of the ultrasonic generator (3) is a conical structure, and the anti-loosening ring (2) is provided with a conical hole that fits into the conical structure.

3. The high mass transfer separation column for a single-rotation countercurrent chromatograph according to claim 1, characterized in that, The spiral groove shape of the power amplifier board (6) fits the outer diameter of the spiral tube (7), and the spiral tube (7) can be embedded in the spiral groove of the power amplifier board (6).

4. A high-mass-transfer separation column for a single-rotation countercurrent chromatograph according to claim 1 or 3, characterized in that, The spiral tube pressure plate (8) is a cross structure with a central hole. A slot communicating with the central hole is opened on the side away from the spiral tube (7). A stop ring (9) is provided above the spiral tube pressure plate (8). The stop ring (9) has a protrusion on its circumference that engages with the slot, so as to fix the stop ring (9) and the spiral tube pressure plate (8) circumferentially, and realize that the spiral tube pressure plate (8) and the spiral tube (7) rotate synchronously.

5. A high-mass-transfer separation column for a single-rotation countercurrent chromatograph according to claim 1, characterized in that, The top plate (10) of the separation column is provided with a strip-shaped mounting hole for the inlet and outlet ends of the spiral tube (7) to extend out.

6. A high-mass-transfer separation column for a single-rotation countercurrent chromatograph according to claim 1 or 5, characterized in that, The inlet and outlet ends of the spiral tube (7) are both connected to a transition assembly; The adapter assembly includes an adapter plate (11), an adapter seat (12), and an adapter (13); the adapter plate (11) is fixed on the top plate (10) of the separation column, and the adapter seat (12) is provided on it. The adapter seat (12) has a flow channel, and the two ends of the flow channel are connected to adapters (13), which are respectively connected to the inlet end or outlet end of the spiral tube (7) and the external feeding pipe.

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