Liquid chromatographic column packing system

Abstract

The utility model provides a liquid chromatographic column packing system, and aims to solve the technical problems that the packing difference of chromatographic columns is large and the packing of each chromatographic column is not uniform in the conventional packing system. The support is divided into the lower support body and the upper support body through the first partition plate. A mounting frame is arranged on the inner top wall of the upper frame body, and a spring is arranged between the outer wall of the mounting frame and the inner wall of the upper frame body. The homogenate tank is mounted on the upper frame body in a penetrating manner along the vertical direction, and a discharge pipeline with a regulating valve is arranged at the bottom end of the homogenate tank. And the motor is mounted in the mounting frame. The installation tank is installed on the lower frame body in a penetrating mode in the vertical direction. The chromatographic column is mounted on the mounting tank in a matched manner, and a second anti-vibration cushion layer is arranged between the chromatographic column and the mounting tank. Wherein one end of the motor is provided with a discharge pipeline, and the other end is connected with the chromatographic column through a hose. Vibration generated by the motor is subjected to multiple buffering through the first anti-vibration cushion layer, the spring and the like in sequence, and the feeding end of the chromatographic column is connected with the hose, so that the influence of the vibration on the filling effect of the chromatographic column is greatly reduced.

Description

Technical Field

[0001] The present application relates to the technical field of liquid chromatography column packing, and in particular to a liquid chromatography column packing system. Background Art

[0002] Fondaparinux sodium is a synthetic heparin pentasaccharide drug that plays a particularly significant role in the prevention and treatment of thromboembolism and venous thrombotic disease in orthopedic joint replacement surgery. The synthetic route for fondaparinux sodium is long, with the number of reaction steps ranging from 50 to over 70. Throughout the entire synthetic process, column purification is often involved multiple times to collect components. If the silica gel columns used have large packing variations, the batch-to-batch variability in purification time will also increase, thereby extending the entire production cycle. Therefore, in order to improve the preparation efficiency of fondaparinux sodium, it is necessary to use chromatographic columns with minimal batch-to-batch packing variations, and each column must also be packed uniformly.

[0003] Currently, the preparation process for industrial chromatography columns is usually as follows: first, silica gel and solvent are evenly mixed in a homogenization tank, and then the mixed liquid in the homogenization tank is pumped into the chromatography column by a high-pressure pump to complete the preparation. During column packing, technicians have found that the following problems may cause the silica gel to be unevenly packed in the chromatography column:

[0004] The vibration generated by the use of the high-pressure pump will be transmitted to the chromatographic column, causing the column to vibrate as well;

[0005] When the high-pressure pump is just started, there will be large fluctuations in the pressure of the slurry pressing against the chromatographic column; during the continuous operation of the high-pressure pump for filling, the pressure in the chromatographic column will also exceed the preset range. Utility Model Content

[0006] The utility model provides a liquid chromatography column packing system to solve the problems raised in the above background technology.

[0007] A liquid chromatography column packing system, comprising:

[0008] The bracket is divided into a lower frame body and an upper frame body by a first partition; a mounting frame is provided on the top wall of the upper frame body, and a spring is provided between the outer wall of the mounting frame and the inner wall of the upper frame body;

[0009] A homogenizing tank is installed vertically through the upper frame, and a discharge pipe with a regulating valve is provided at the bottom end thereof;

[0010] The transmission assembly includes a motor and a hose; the motor is installed in the mounting frame;

[0011] The mounting assembly includes a mounting tank and a chromatographic column; the mounting tank is vertically installed through the lower frame; the chromatographic column is matched and installed in the mounting tank, and a second vibration-damping pad is provided between the mounting tank and the chromatographic column;

[0012] Wherein, one end of the motor is equipped with the discharge pipe, and the other end is connected to the chromatographic column through the hose.

[0013] Furthermore, an installation groove is formed on the inner side wall of the installation frame, and a first vibration-damping pad is installed in the installation groove.

[0014] Furthermore, a pressure sensor is provided on the inner wall of the hose; a controller is also installed on the mounting frame; an input end of the controller is electrically connected to the pressure sensor, and an output end thereof is electrically connected to the motor and the regulating valve respectively.

[0015] Furthermore, the inner cavity of the installation tank is divided into an upper cavity and a lower cavity in sequence through a second partition; the second partition is provided with a connecting hole along the vertical direction.

[0016] Furthermore, a vacuum pipe communicating with the lower cavity is provided on the side wall of the installation tank; the vacuum pipe is provided with a vacuum valve and is externally connected to a vacuum pump.

[0017] Furthermore, a waste liquid discharge pipe is provided at the bottom end of the lower cavity, and the waste liquid discharge pipe is sealed by a flange.

[0018] Furthermore, the lower frame also includes multiple vertical plates and inclined plates; multiple vertical plates are installed on the bottom end of the first partition along the circumference of the cross-section of the bottom end of the first partition; one end of the inclined plate is connected to a vertical plate, and the other end is connected to the first partition.

[0019] Furthermore, a liquid inlet pipe is provided at the top of the chromatographic column, and the hose is matched and connected inside the liquid inlet pipe; a liquid outlet pipe is provided at the bottom of the chromatographic column, and the liquid outlet pipe passes through the connecting hole and extends to the lower cavity.

[0020] Compared with the prior art, the beneficial effects of the present invention are:

[0021] (1) The vibration generated by the motor is buffered by the first vibration damping pad, the spring, and the second vibration damping pad in sequence, and the feed end of the chromatographic column is connected to the hose, which greatly reduces the influence of the vibration on the filling effect of the chromatographic column and is conducive to the preparation of a uniformly filled chromatographic column.

[0022] (2) A pressure sensor is provided at the hose, which is electrically connected to the controller. The controller controls the motor and regulating valve to control the pressure fluctuation and pressure range in the column during the column filling process. This realizes the automation of stable column filling, improves the column filling efficiency, and ensures that each column has a stable filling effect between batches. BRIEF DESCRIPTION OF THE DRAWINGS

[0023] In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the following briefly introduces the drawings required for use in the embodiments or the description of the prior art. Obviously, the drawings described below are only some embodiments of the present application. For ordinary technicians in this field, other drawings can be obtained based on these drawings without any creative work.

[0024] Figure 1 This is a schematic structural diagram of a liquid chromatography column packing system according to an embodiment of the present application;

[0025] Figure 2 This is a partial enlarged view of A of a liquid chromatography column packing system according to an embodiment of the present application.

[0026] Reference numerals:

[0027] 10. Upper frame; 11. First partition; 12. Vertical plate; 13. Mounting frame; 131. First vibration damping pad; 14. Spring; 15. Inclined plate;

[0028] 20. Homogenizer tank; 21. Discharge pipe;

[0029] 30. Motor; 32. Hose; 33. Pressure sensor; 34. Controller; 35. Control valve;

[0030] 4. Mounting tank; 40. Second partition; 41. Lower cavity; 42. Chromatographic column; 421. Liquid outlet pipe of chromatographic column; 43. Second vibration-damping pad; 44. Vacuum pipe; 45. Waste liquid discharge pipe; 451. Flange. DETAILED DESCRIPTION

[0031] Hereinafter, only certain exemplary embodiments are briefly described. As will be appreciated by those skilled in the art, the described embodiments may be modified in various ways without departing from the spirit or scope of the present invention. Therefore, the drawings and description are to be regarded as illustrative in nature and not restrictive.

[0032] In the description of the present invention, it should be understood that the terms "center", "thickness", "up", "down", "top", "bottom", "inside", "outside", "vertical", "circumferential", etc., indicating the orientation or position relationship, are based on the orientation or position relationship shown in the accompanying drawings, or are the orientation or position relationship in which the product of the present invention is usually placed when in use, or are the orientation or position relationship commonly understood by those skilled in the art. They are only for the convenience of describing the present invention and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore cannot be understood as a limitation on the present invention.

[0033] Furthermore, the terms "first" and "second" are used for descriptive purposes only and should not be construed as indicating or implying relative importance or implicitly specifying the number of the technical features being referred to. Thus, a feature specified as "first" or "second" may explicitly or implicitly include one or more of such features. In the description of this utility model, "plurality" means two or more, unless otherwise specifically defined.

[0034] In this utility model, unless otherwise expressly specified or limited, the terms "installed," "connected," "connect," "fixed," etc. should be understood in a broad sense. For example, they can refer to fixed connection, detachable connection, or integration; mechanical connection, electrical connection, or communication; direct connection or indirect connection through an intermediate medium; internal communication between two components or interaction between two components. For those skilled in the art, the specific meanings of the above terms in this utility model can be understood according to specific circumstances.

[0035] In the present invention, unless otherwise expressly specified or limited, a first feature being "above" or "below" a second feature may include the first and second features being in direct contact, or may include the first and second features being in contact not directly but through another feature between them. Moreover, a first feature being "above," "above," and "above" a second feature may include the first feature being directly above or obliquely above the second feature, or may simply mean that the first feature is higher in level than the second feature. A first feature being "below," "below," and "below" a second feature may include the first feature being directly below or obliquely below the second feature, or may simply mean that the first feature is lower in level than the second feature.

[0036] The disclosure below provides many different embodiments or examples for realizing different structures of the present invention. In order to simplify the disclosure of the present invention, the components and settings of specific examples are described below. Of course, they are merely examples and are not intended to limit the present invention. In addition, the present invention may repeat reference numbers and / or reference letters in different examples. Such repetition is for the purpose of simplicity and clarity and does not in itself indicate the relationship between the various embodiments and / or settings discussed. In addition, the present invention provides examples of various specific processes and materials, but a person of ordinary skill in the art will recognize the application of other processes and / or the use of other materials.

[0037] The embodiments of the present invention are described in detail below with reference to the accompanying drawings.

[0038] The present invention provides a liquid chromatography column packing system. Figure 1-Figure 2 , which includes a frame, a homogenization tank 20, a transmission component and a mounting component.

[0039] Specifically,

[0040] The frame includes a lower frame and an upper frame 10. The upper frame 10 is installed on the outer top end of the lower frame.

[0041] The lower frame 10 comprises a first partition 11, multiple vertical panels 12, and an inclined panel 15. A through-hole is provided in the center of the first partition 11. Multiple vertical panels 12 are mounted on the bottom end of the first partition 11 along the circumference of its cross-section to support the bottom end. To further enhance the stability of the lower frame, one end of the inclined panel 15 is connected to a vertical panel 12, and the other end of the inclined panel 15 is connected to the first partition 11.

[0042] The upper frame 10 is a hollow rectangular parallelepiped with a sealed top. A mounting bracket 13 is mounted on the inner top of the upper frame 10, creating a space between the mounting bracket 13 and the inner top wall of the upper frame 10 for mounting components. A mounting groove is defined in the inner sidewall of the mounting bracket 13, into which a first vibration-damping pad 131 is mounted. A spring 14 is installed between the outer sidewall of the mounting bracket 13 and the inner sidewall of the upper frame 10. The upper frame 10 can be connected to the outer top of the lower frame via bolts.

[0043] The homogenization tank 20 contains the silica gel suspension to be loaded into the column. A discharge pipe 21 is located at the bottom of the homogenization tank 20. This discharge pipe 21 is equipped with a regulating valve 35 to control the discharge flow rate of the homogenization tank 20. After the homogenization tank 20 passes through the top of the upper frame 10, the side walls of the homogenization tank 20 are mounted on the top of the upper frame.

[0044] The transmission component includes a motor 30 and a hose 32. The motor 30 is installed in the accommodation space of the upper frame 10. The liquid inlet end of the motor 30 is connected to the discharge pipe 21 of the homogenization tank 20, and the liquid outlet end thereof is installed with a hose 32, so that the slurry in the homogenization tank 20 can be pressed outward by the motor 30. Among them, the vibration transmitted to the mounting frame 13 due to the operation of the motor 30 can be buffered by the first vibration-damping pad 131, and then the vibration transmitted from the mounting frame 13 to the upper frame 10 is buffered by the spring 14, and the overall vibration of the frame is reduced through double vibration reduction. At the same time, a pressure sensor 33 is provided on the inner wall of the hose 32. The controller 34 is arranged at the bottom end of the mounting frame 13, and the input end of the controller 34 is electrically connected to the pressure sensor 33, and the output end thereof is electrically connected to the motor 30 and the regulating valve 35 respectively. When the controller 34 receives a pressure signal from the pressure sensor 33 that fluctuates greatly, it controls the motor power to maintain stable pressurization of the hose 32; when the pressure sensed by the pressure sensor 33 is greater than or less than the set pressure range, the controller 34 processes the corresponding pressure signal received and controls the regulating valve 35 to adjust the discharge flow rate of the slurry tank 20.

[0045] The mounting assembly is mounted on the lower frame and includes a mounting tank 4 and a chromatographic column 42. After the chromatographic column 42 is mounted in the mounting tank 4, the liquid inlet end of the chromatographic column 42 is connected to the hose 32, thereby enabling the slurry in the homogenization tank 20 to be pressed toward the chromatographic column 42 by the motor 30.

[0046] The mounting tank 4 is matched with the through hole of the first partition 11, that is, the outer diameter of the mounting tank 4 is equal to the diameter of the through hole, so that the mounting tank 4 can be installed through the lower frame. The inner cavity of the mounting tank 4 is divided into an upper cavity and a lower cavity 41 in sequence through the second partition 40. The second partition 40 is provided with a connecting hole from top to bottom, and the upper cavity and the lower cavity 41 are communicated through the connecting hole. A second vibration-damping pad 43 is installed on the side wall of the upper cavity. A vacuum pipe 44 is provided on the side wall of the mounting tank to communicate with the lower cavity 41. The vacuum pipe 44 is connected to a vacuum pump, and the air in the inner cavity can be discharged through the vacuum pump. A vacuum valve is provided on the vacuum pipe 44. A waste liquid discharge pipe 45 is provided at the bottom end of the lower cavity 41, and the waste liquid discharge pipe 45 is sealed by a flange 451.

[0047] The chromatographic column 42 has a liquid inlet pipe at its top and a liquid outlet pipe at its bottom. The chromatographic column 42 is matched and installed in the upper cavity so that the second vibration-damping pad 43 installed in the upper cavity can enclose the chromatographic column 42 therein. The liquid inlet pipe of the chromatographic column 42 is matched and connected to the hose 32. That is, the outer diameter of the bottom end of the hose 32 is equal to the inner diameter of the liquid inlet pipe, so that the hose 32 located in the liquid inlet pipe can fit the inner wall of the liquid inlet pipe, thereby preventing bubbles from entering the chromatographic column 42 during filling. When the slurry in the homogenization tank 20 is pressed against the chromatographic column 42 by the motor 30 for filling, the hose 32 is connected via the liquid inlet pipe to reduce the impact of vibration on the chromatographic column 42. At the same time, the second vibration-damping pad 43 weakens the vibration transmitted to the chromatographic column 42 by the installation tank 4, which is beneficial to the uniformity of the filling of the chromatographic column 42. In addition, the liquid outlet pipe 421 of the chromatographic column extends through the connecting hole to the lower cavity 41, so that the waste liquid flowing out of the chromatographic column 42 during filling can be collected in the lower cavity 41.

[0048] Based on the above embodiments, the working principle of this application is as follows:

[0049] Before filling, open the vacuum valve and start the vacuum pump to remove the air in the lower cavity and the chromatographic column 42 in an empty column state.

[0050] During filling, the vacuum pump is turned off and the motor 30 is started, allowing the slurry in the homogenization tank 20 to be pressed against the chromatographic column 42. The resulting waste liquid is collected in the lower cavity 41. When the motor 30 is first started, the homogenization tank 20 is prone to experiencing large pressure fluctuations. This pressure signal is detected by a pressure sensor 33 located in the hose 32 and transmitted to a controller 34 to control the motor power to maintain stable pressurization in the chromatographic column 42. During the operation of the motor 30, if the pressure in the hose 32 exceeds or falls below the set pressure range, the controller 34 further controls the regulating valve 35 to achieve automated and stable filling of the chromatographic column 42, thereby improving column filling efficiency.

[0051] After filling is completed, the motor 30 is turned off, the flange 451 and the discharge valve are opened, and the waste liquid collected in the lower cavity 41 is discharged.

[0052] Based on the above embodiments, the advantages of this application are:

[0053] (1) The vibration generated by the motor 30 is buffered by the first vibration-damping pad 131, the spring 14, and the second vibration-damping pad 43 in sequence, and the liquid inlet end 421 of the chromatographic column is connected to the hose 32, which greatly reduces the influence of the vibration on the filling effect of the chromatographic column 42, and is conducive to the preparation of a uniformly filled chromatographic column 42.

[0054] (2) A pressure sensor 33 is provided at the hose 32, which is electrically connected to the controller 34. The controller 34 controls the motor 30 and the regulating valve 35 to control the pressure fluctuation and pressure range in the column during the filling process of the chromatographic column 34. This realizes the automation of stable filling of the chromatographic column 34, improves the efficiency of column filling, and ensures that each chromatographic column 34 has a stable filling effect between batches.

Claims

1. A liquid chromatography column packing system, characterized in that: The column packing system comprises: The bracket is divided into a lower frame body and an upper frame body by a first partition; a mounting frame is provided on the top wall of the upper frame body, and a spring is provided between the outer wall of the mounting frame and the inner wall of the upper frame body; A homogenizing tank is installed vertically through the upper frame, and a discharge pipe with a regulating valve is provided at the bottom end thereof; The transmission assembly includes a motor and a hose; the motor is installed in the mounting frame; The mounting assembly includes a mounting tank and a chromatographic column; the mounting tank is vertically installed through the lower frame; the chromatographic column is matched and installed in the mounting tank, and a second vibration-damping pad is provided between the mounting tank and the chromatographic column; Wherein, one end of the motor is equipped with the discharge pipe, and the other end is connected to the chromatographic column through the hose.

2. The liquid chromatography column packing system according to claim 1, characterized in that: A pressure sensor is provided on the inner wall of the hose; a controller is also installed on the mounting frame; an input end of the controller is electrically connected to the pressure sensor, and an output end thereof is electrically connected to the motor and the regulating valve respectively.

3. The liquid chromatography column packing system according to claim 1, characterized in that: An installation groove is formed on the inner side wall of the installation frame, and a first vibration-damping pad is installed in the installation groove.

4. The liquid chromatography column packing system according to claim 1, characterized in that: The inner cavity of the installation tank is divided into an upper cavity and a lower cavity in sequence through a second partition plate; the second partition plate is provided with a connecting hole along the vertical direction.

5. The liquid chromatography column packing system according to claim 4, characterized in that: A vacuum pipe communicating with the lower cavity is provided on the side wall of the installation tank; the vacuum pipe is provided with a vacuum valve and is externally connected to a vacuum pump.

6. The liquid chromatography column packing system according to claim 4, characterized in that: A waste liquid discharge pipe is provided at the bottom end of the lower cavity, and the waste liquid discharge pipe is sealed by a flange.

7. The liquid chromatography column packing system according to claim 4, characterized in that: The lower frame also includes multiple vertical plates and inclined plates; multiple vertical plates are installed on the bottom end of the first partition along the circumference of the cross-section of the bottom end of the first partition; one end of the inclined plate is connected to a vertical plate, and the other end is connected to the first partition.

8. The liquid chromatography column packing system according to claim 7, characterized in that: The top of the chromatographic column is provided with a liquid inlet pipe, and the hose is matched and connected to the liquid inlet pipe to prevent bubbles from entering during filling; the bottom of the chromatographic column is provided with a liquid outlet pipe, and the liquid outlet pipe passes through the connecting hole and extends to the lower cavity.

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