A high pressure liquid medium sampling device

Abstract

The application discloses a high-pressure liquid-phase medium sampling device and relates to the technical field of six-way sampling valves.The application aims at the problem that the existing six-way sampling valve is prone to sealing surface failure and medium pressure reverse transmission leading to valve damage in high-pressure liquid-phase medium sampling;the impact of high-pressure liquid-phase medium is eliminated through a flow path buffer assembly, flow path matching surface damage is avoided, reverse conduction of overpressure medium pressure is blocked, permanent damage of the valve is prevented, medium flow stability of constant volume sampling is ensured;relying on an axial sealing assembly, circumferential rotation is converted into axial movement, axial and radial double sealing pre-tightening of the flow path matching surface is realized, the problem of sealing surface failure is solved, sampling contamination is avoided, and sampling purity is ensured;through linkage of the core rotating rod, flow path switching, sealing pre-tightening and other actions, the structure is compact, the high-pressure leakage-free advantage of the six-way sampling valve is retained, the device is suitable for high-pressure, microliter constant volume and multi-phase corrosive liquid-phase medium sampling scenes, and the device running stability and scene adaptability are improved.

Description

Technical Field

[0001] This invention relates to the field of six-way injection valve technology, and more specifically to a high-pressure liquid phase medium sampling device. Background Technology

[0002] The six-way injection valve is a core sampling component in high-performance liquid chromatography (HPLC), high-pressure preparative liquid chromatography, and online sampling of high-performance liquid chromatography processes. Its core advantage is that it can achieve leak-free flow path switching and precise volume sampling under high-pressure conditions. It is suitable for the typical working pressure of 10~40MPa, μL-level volume sampling, and multiphase / corrosive liquid media.

[0003] Referring to a micro-sampling device based on a six-way valve disclosed in patent application number 202122250543.7, key components such as a quantitative ring are placed inside the six-way valve. Given that the valve body itself lacks the capacity to accommodate the rated volume, the built-in quantitative ring cannot be effectively extended or even replaced under different sampling requirements, making it difficult to guarantee its volume accuracy, which directly affects the sampling accuracy.

[0004] For example, the description of an autosampler for a liquid chromatograph disclosed in patent application number 201710736196.4 improves the sampling requirement structure of the quantitative loop by designing it to change the injection volume through a syringe. However, existing quantitative loops can also achieve sampling by partial liquid filling when the sampling requirement is determined. Therefore, although the physical volume of the quantitative loop is not changeable, accurate sampling can be achieved without replacing the quantitative loop by partial liquid filling, thereby avoiding the problem of inaccurate sampling that may be caused by pushing with a "syringe".

[0005] However, while existing high-pressure six-way injection valves can meet basic sampling requirements, they are prone to sealing failure during long-term, high-frequency rotation switching (friction between rotor and stator ceramic surfaces) or when the liquid medium contains microparticles. This can lead to contamination of the high-pressure liquid medium sample. Alternatively, when the main liquid pressure exceeds the limit, the pressure can be transmitted back to the valve, causing permanent damage. Therefore, the problems that need to be solved by existing high-pressure six-way injection valves are as described above. To ensure sampling accuracy and effective sealing, this application proposes a solution. Summary of the Invention

[0006] The purpose of this invention is to provide a high-pressure liquid phase medium sampling device to solve the problems mentioned in the background art.

[0007] The objective of this invention can be achieved through the following technical solution: a high-pressure liquid phase medium sampling device, including a valve seat, a shaft seal is provided inside the valve seat, a rotating rod is installed on the shaft seal, a rotating core seat is connected to the upper end of the rotating rod, and an arc-shaped flow channel distributed at a 60° angle to each other is opened on the rotating core seat;

[0008] The stator is mounted on the valve seat and has a flow hole that is smoothly connected to the arc-shaped flow channel. An interface cover is installed on the stator corresponding to the opening of the flow hole.

[0009] A flow path buffer assembly includes a flow path buffer sheet disposed inside the interface cover. The flow path buffer sheet is distributed in an umbrella shape and an annular spring assembly connected to the inner wall of the interface cover is installed on the upper end of the outer ring side.

[0010] The configuration is further defined as follows: an axial sealing plate is installed on the rotating core seat, and an axial sealing assembly is provided at the outer end of the axial sealing plate. The axial sealing assembly includes sealing spring rings, which are stacked in a ring and have deformation grooves staggered at their ends from bottom to top.

[0011] The axial sealing plate is further configured such that a lead screw is threadedly connected to the upper end of the axial sealing plate, and the lead screw is fixedly connected to the top of the stator.

[0012] The interface cover is further configured such that an interface seat that mates with a flow hole is installed on the outer side of the interface cover, a fluid inlet is provided at the lower end of the interface cover that fits against the bottom of the unfolded flow path buffer sheet, and a tangential flow channel is provided on the top of the interface cover corresponding to the flow path buffer sheet.

[0013] The valve seat is further configured such that a quantitative ring, a sample flow path tube, and a waste liquid tube are connected to the valve seat via an interface cover.

[0014] The method is further configured such that the metering ring is a hollow capillary channel with a fixed volume, and the metering ring is connected to two vertically corresponding interface caps for fixed-volume sampling of high-pressure liquid media.

[0015] The interface cover is further configured to connect the sample flow path inlet, sample flow path outlet, quantitative loop inlet, quantitative loop outlet, manual injection port, and waste liquid port, respectively. The quantitative loop inlet and quantitative loop outlet are used to connect the quantitative loop, the waste liquid port is used to connect the waste liquid tube, and the sample flow path inlet and sample flow path outlet are used to connect the sample flow path tube.

[0016] A further feature is provided: the top of the stator is provided with an indicator arrow for indicating the connection between the two arc-shaped flow channels and two sets of flow holes.

[0017] The present invention has the following beneficial effects:

[0018] 1. This invention addresses the technical problem of existing six-way sampling valves being prone to sealing surface failure and reverse pressure transmission leading to valve damage during high-pressure liquid phase sampling. It utilizes a flow path buffer assembly to mitigate the impact of high-pressure liquid phase media, preventing damage to the flow path mating surfaces and simultaneously blocking the reverse transmission of overpressure, thus preventing permanent valve damage and ensuring the stability of medium flow during constant-volume sampling. Furthermore, it employs an axial sealing assembly to convert circumferential rotation into axial movement, achieving axial and radial double sealing pre-tightening of the flow path mating surfaces, solving the sealing surface failure problem, preventing sample contamination, and ensuring sample purity.

[0019] 2. This invention adopts an external quantitative ring design, which not only ensures volume accuracy but also allows for convenient disassembly and replacement as needed, adapting to diverse sampling requirements. Furthermore, through the core rotating rod linkage flow path switching and sealing pre-tightening actions, the structure is compact and retains the high-pressure leak-free advantage of the six-way injection valve, making it suitable for high-pressure, micro-volume constant-volume and multiphase corrosive liquid media sampling scenarios, improving the device's operational stability and scenario adaptability. Attached Figure Description

[0020] To more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0021] Figure 1 This is a schematic diagram of the structure of the present invention;

[0022] Figure 2 This is a bottom view diagram of the present invention;

[0023] Figure 3 This is a top view of the present invention;

[0024] Figure 4 This is a schematic diagram of the deflection of the present invention;

[0025] Figure 5 This is a side sectional view of the present invention;

[0026] Figure 6 This is a partial structural cross-sectional view of the present invention;

[0027] Figure 7 This is a partial structural diagram of the sealing spring ring of the present invention;

[0028] Figure 8 This is a schematic diagram of the installation of the flow path buffer sheet of the present invention;

[0029] Figure 9 This is a cross-sectional schematic diagram of the installation structure of the flow path buffer sheet of the present invention.

[0030] In the diagram: 1. Valve seat; 2. Stator; 3. Interface cover; 4. Metering ring; 5. Sample flow path tube; 6. Waste liquid tube; 7. Rotating rod; 8. Indicating arrow; 9. Arc-shaped flow channel; 10. Flow hole; 11. Shaft seal; 12. Rotating core seat; 13. Axial sealing plate; 14. Lead screw; 15. Flow path buffer plate; 16. Sealing spring ring; 17. Deformation groove; 18. Interface seat; 19. Annular spring assembly; 20. Shear flow channel. Detailed Implementation

[0031] The technical solution of the present invention will be clearly and completely described below with reference to the embodiments. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the scope of protection of the present invention.

[0032] Example 1

[0033] To address the technical problems of existing six-way injection valves, such as sealing surface failure and reverse pressure transmission leading to valve damage during high-pressure liquid sampling, as well as the difficulty in guaranteeing the accuracy of the built-in volume of the metering loop, the following technical solutions are proposed:

[0034] Reference Figure 1 - Figure 9 As shown, in this embodiment, a high-pressure liquid medium sampling device includes a valve seat 1, a shaft seal 11 is provided inside the valve seat 1, a rotating rod 7 is installed on the shaft seal 11, and a rotating core seat 12 is connected to the upper end of the rotating rod 7. The rotating core seat 12 has arc-shaped flow channels 9 distributed at 60° angles to each other. When the rotating rod 7 rotates around the shaft seal 11 in a circumferential direction, it synchronously drives the rotating core seat 12 to rotate, so that the arc-shaped flow channels 9 at 60° angles to each other on the rotating core seat 12 and the flow holes 10 on the stator 2 are switched on and off, realizing the basic switching action of the flow path.

[0035] Stator 2 is mounted on valve seat 1. Stator 2 has a flow hole 10 that is smoothly connected to the arc-shaped flow channel 9. An interface cover 3 is installed on stator 2 corresponding to the opening of the flow hole 10.

[0036] The flow path buffer assembly includes a flow path buffer plate 15 disposed inside the interface cover 3. The flow path buffer plate 15 is distributed in an umbrella shape and an annular spring assembly 19 connected to the inner wall of the interface cover 3 is installed on the upper end of the outer ring side.

[0037] When the high-pressure liquid medium enters through the fluid inlet of the interface cover 3, the high-pressure impact force of the medium acts on the bottom of the umbrella-shaped flow path buffer plate 15, causing the flow path buffer plate 15 to undergo elastic deformation and press the annular spring assembly 19 to the top. The annular spring assembly 19 generates a reverse elastic force, which, together with the deformation of the flow path buffer plate 15, dissipates the high-pressure impact of the medium. The buffered medium is guided upward along the umbrella surface of the flow path buffer plate 15 and smoothly enters the flow hole 10 through the tangential flow channel 20, avoiding direct impact of the medium on the mating surface of the flow hole 10 and the arc-shaped flow channel 9.

[0038] Reference Figure 5 and Figure 6 As shown, an axial sealing plate 13 is installed on the rotating core seat 12. An axial sealing assembly is provided at the outer end of the axial sealing plate 13. The axial sealing assembly includes a sealing spring ring 16. The sealing spring rings 16 are stacked in a ring and the ends are staggered with deformation grooves 17 from bottom to top. A lead screw 14 is threaded to the upper end of the axial sealing plate 13. The lead screw 14 is fixedly connected to the top of the stator 2.

[0039] Simultaneously, the circumferential rotation of the rotating core seat 12 drives the axial sealing plate 13 to move synchronously in the circumferential direction. The threaded engagement between the lead screw 14 and the axial sealing plate 13 converts the circumferential rotation into the axial linear pressing motion of the axial sealing plate 13. The axial sealing plate 13 drives the sealing spring ring 16 to bear the axial pressure. Due to the annular stacked structure and the deformation grooves 17 staggered at the ends, the sealing spring ring 16 contracts axially and expands radially under the axial pressure, achieving axial and radial double sealing pre-tightening of the mating surface between the rotating core seat 12 and the stator 2, ensuring the sealing performance at the flow path connection.

[0040] An interface seat 18 that mates with the flow hole 10 is installed on the outer side of the interface cover 3. A fluid inlet is provided at the lower end of the interface cover 3 to fit the bottom of the unfolded flow path buffer plate 15. A tangential flow channel 20 is provided on the top of the interface cover 3 corresponding to the flow path buffer plate 15.

[0041] Basic Principle: This invention improves the structure of existing six-way sampling valves to avoid sampling contamination caused by sealing surface failure during high-pressure liquid sampling. On one hand, the combined use of a flow path buffer assembly and an axial sealing assembly effectively buffers the high-pressure impact of the liquid medium during sampling, reducing the impact on the metering ring and interface. This eliminates the direct impact of the high-pressure medium on the flow hole and arc-shaped flow channel connection surface, and effectively prevents the overpressure medium in the main liquid path from being transmitted back to the valve body, fundamentally preventing permanent damage to the valve components.

[0042] On the other hand, during the flow path switching process, the axial linear motion of the lead screw 14 and the axial sealing plate 13 drives the pressing process of the sealing spring ring 16, which enables the sealing spring ring 16 to undergo bidirectional reciprocating deformation along the axial and radial directions. This effectively pre-tightens the sealing surface of the connection between the flow hole and the arc-shaped flow channel, especially ensuring the effective sealing of the connection surface when the high-pressure medium is injected into the metering ring 4 through the connecting flow path. With the effective combination of the two, the axial seal combined with the radial seal effectively seals the connection surface of the loop flow path, avoiding the risk of leakage caused by the direct impact of the high-pressure medium and ensuring the accurate sampling of the high-pressure liquid phase medium.

[0043] Example 2

[0044] Reference Figure 1 - Figure 9 As shown, this embodiment is based on embodiment one, and further optimizes the structure in embodiment one; including a metering ring 4, a sample flow path tube 5 and a waste liquid tube 6 connected to the valve seat 1 through interface covers 3 respectively. The metering ring 4 is a hollow capillary flow channel with a fixed volume. The metering ring 4 is connected to two vertically corresponding interface covers 3 for fixed-volume sampling of high-pressure liquid phase medium. The interface covers 3 are respectively used to connect the sample flow path inlet, sample flow path outlet, metering ring 4 inlet, metering ring 4 outlet, manual injection port and waste liquid port. The metering ring 4 inlet and metering ring 4 outlet are respectively used to connect the metering ring 4, the waste liquid port is used to connect the waste liquid tube 6, and the sample flow path inlet and sample flow path outlet are used to connect the sample flow path tube 5.

[0045] The top of the stator 2 is provided with an indicator arrow 8, which is used to indicate the connection between the two arc-shaped flow channels 9 and the two sets of flow holes 10.

[0046] Basic principle: When the arc-shaped flow channel 9 is connected to the flow hole 10 corresponding to the sample flow path inlet and the quantitative loop 4 inlet, the high-pressure liquid phase medium, after being buffered by the flow path buffer assembly, enters the quantitative loop 4 through the sample flow path tube 5 until the quantitative loop 4 is filled with the medium, completing the μL-level constant volume sampling action; when the arc-shaped flow channel 9 rotates to be connected to the flow hole 10 corresponding to the quantitative loop 4 outlet and the subsequent detection flow path, the main pressure of the high-pressure liquid phase medium pushes the constant volume medium in the quantitative loop 4 into the subsequent detection flow path, realizing the delivery of the sampling medium; when the arc-shaped flow channel 9 is connected to the flow hole 10 corresponding to the waste liquid outlet, excess medium, residual medium or waste medium in the flow path can enter the waste liquid tube 6 through the flow hole 10 and be discharged, realizing the waste liquid drainage of the flow path;

[0047] Meanwhile, the manual injection port can be independently connected to the arc-shaped flow channel 9, and manual injection can be completed by manually injecting the sample. At this time, the rotation of the arc-shaped flow channel 9 can realize the pairing of the manual injection flow path with the quantitative loop 4 and the detection flow path to complete the manual volume-fixed sampling. Moreover, the externally connected quantitative loop 4 can be directly disassembled and replaced according to the sampling volume requirements to adapt to different volume-fixed sampling scenarios.

[0048] Example 3

[0049] Reference Figure 1 - Figure 9 As shown, this embodiment combines the technical content of Embodiment 1 and Embodiment 2 to form the following usage method:

[0050] Step 1: First, according to the sampling volume requirements of the high-pressure liquid medium, select a quantitative ring 4 of suitable specifications and connect its two ends to the two vertically paired interface caps 3 on the valve seat 1 to complete the assembly of the quantitative flow path. At the same time, connect the sample flow path tube 5 and the waste liquid tube 6 to the interface caps 3 of the corresponding functions to complete the overall flow path construction of the device.

[0051] Step 2: Then start the high-pressure liquid medium delivery system. The medium enters the interface cover 3 corresponding to the sample flow path inlet through the sample flow path tube 5, and smoothly enters the flow hole 10 of the stator 2 through the tangential flow channel 20. Manually rotate the rotating rod 7. The rotating rod 7 drives the rotating core seat 12 to rotate circumferentially around the shaft seal 11. Observe and adjust the connection status of the arc-shaped flow channel 9 through the indicator arrow 8 on the top of the stator 2 so that the arc-shaped flow channel 9 is precisely matched with the flow hole 10 corresponding to the sample flow path and the quantitative ring 4. The medium enters the quantitative ring 4 with a fixed volume under the pressure of the main road, and the fixed-volume sampling is completed.

[0052] Step 3: In step 2, the axial sealing plate 13 rotates with the rotating core seat 12, and axial clamping is achieved through the threaded transmission of the lead screw 14, which drives the sealing spring ring 16 to complete the axial and radial pre-tightening of the sealing surface; continue to rotate the rotating rod 7 to adjust the angle of the rotating core seat 12, so that the arc-shaped flow channel 9 switches to the flow hole 10 corresponding to the quantitative ring 4 and the subsequent detection flow path. The high-pressure medium in the main road pushes the constant volume medium in the quantitative ring 4 into the detection flow path to complete the sampling and delivery; if there is excess medium in the flow path or it is necessary to drain the residual medium, continue to rotate the rotating rod 7 to connect the arc-shaped flow channel 9 with the flow hole 10 corresponding to the waste liquid port, and discharge the waste medium from the waste liquid pipe 6;

[0053] Step 4: When manual sampling is required, shut off the media delivery of the automatic flow path and inject the sample through the manual injection port. Rotate the rotating rod 7 to connect the manual injection port with the quantitative loop 4 and the detection flow path through the arc-shaped flow channel 9, and complete the manual volume-fixing sampling operation. During the entire use of the device, the flow path switching, sealing pre-tightening, and high-pressure buffering actions are carried out simultaneously until the sampling operation is completed. Then shut off the media delivery system to complete the device's usage process.

[0054] The results of the solution are as follows:

[0055] The sampling device uses the circumferential rotation of the rotating rod 7 around the shaft seal 11 as its core power source, which synchronously drives the flow path switching movement of the rotating core seat 12 and the axial sealing pre-tightening movement of the axial sealing plate 13 and the lead screw 14. The pressure of the high-pressure liquid medium itself serves as the triggering power for the flow path buffer assembly, enabling the flow path buffer plate 15 and the annular spring assembly 19 to complete the high-pressure buffering action. All movements are linked and coordinated synchronously, achieving flow path switching and constant volume sampling while completing sealing pre-tightening and high-pressure buffering, ensuring the stable operation of the device under high-pressure conditions.

[0056] In summary, this invention, on the one hand, sets up an umbrella-shaped flow path buffer plate 15 and an annular spring group 19 inside the interface cover 3 to form a flow path buffer assembly. The pressure of the high-pressure liquid phase medium itself triggers the deformation of the flow path buffer plate 15 and the elastic expansion and contraction of the annular spring group 19, which effectively dissipates the high-pressure impact of the medium. This not only avoids the damage to the sealing surface caused by the high-pressure medium directly impacting the mating surface of the flow hole 10 and the arc-shaped flow channel 9, but also prevents the overpressure medium pressure of the main liquid phase path from being transmitted back to the valve seat 1 and the stator 2, fundamentally preventing permanent damage to the valve components due to overpressure. At the same time, the buffered medium smoothly enters the flow path, ensuring the flow stability of the medium during constant volume sampling.

[0057] On the other hand, the axial sealing assembly is formed by the axial sealing plate 13, the lead screw 14 and the stacked sealing spring rings 16 on the rotating core seat 12. The circumferential rotation is converted into the axial linear motion of the axial sealing plate 13 by the linkage of the rotating rod 7. Under axial pressure, the sealing spring rings 16 achieve axial contraction and radial expansion by means of the staggered deformation grooves 17, and complete the axial and radial double sealing pre-tightening of the mating surface between the rotating core seat 12 and the stator 2. This effectively solves the problem of sealing surface failure that occurs in existing devices when there are long-term high-frequency rotation switching or when the liquid medium contains microparticles. It also avoids the doping phenomenon in the high-pressure liquid medium sampling process and ensures the purity of the sample.

[0058] The above description is merely an example and illustration of the structure of the present invention. Those skilled in the art can make various modifications or additions to the specific embodiments described, or use similar methods to replace them, as long as they do not deviate from the structure of the invention or exceed the scope defined in the claims, all of which should fall within the protection scope of the present invention.

[0059] In the description of this specification, references to terms such as "an embodiment," "example," and "specific example" indicate that a specific feature, structure, material, or characteristic described in connection with that embodiment or example is included in at least one embodiment or example of the invention. In this specification, illustrative expressions of the above terms do not necessarily refer to the same embodiment or example. Furthermore, the specific features, structures, materials, or characteristics described may be combined in any suitable manner in one or more embodiments or examples.

[0060] The preferred embodiments of the present invention disclosed above are merely illustrative of the invention. These preferred embodiments do not exhaustively describe all details, nor do they limit the invention to specific implementations. Clearly, many modifications and variations can be made based on the content of this specification. This specification selects and specifically describes these embodiments to better explain the principles and practical applications of the invention, thereby enabling those skilled in the art to better understand and utilize the invention. The invention is limited only by the claims and their full scope and equivalents.

Claims

1. A high-pressure liquid phase medium sampling device, characterized in that, include: Valve seat (1), the valve seat (1) is provided with a shaft seal (11), a rotating rod (7) is installed on the shaft seal (11), the upper end of the rotating rod (7) is connected to a rotating core seat (12), and an arc-shaped flow channel (9) distributed at a 60° angle to each other is opened on the rotating core seat (12). Stator (2), the stator (2) is disposed on valve seat (1), the stator (2) is provided with a flow hole (10) that is smoothly connected to the arc flow channel (9), the stator (2) is provided with an interface cover (3) corresponding to the opening of the flow hole (10), the outside of the interface cover (3) is provided with an interface seat (18) that cooperates with the flow hole (10), the lower end of the interface cover (3) is provided with a fluid inlet that fits against the bottom of the unfolded flow path buffer plate (15), and the top of the interface cover (3) is provided with a tangential flow channel (20). The flow path buffer assembly includes a flow path buffer plate (15) disposed inside the interface cover (3). The flow path buffer plate (15) is distributed in an umbrella shape and an annular spring assembly (19) connected to the inner wall of the interface cover (3) is installed on the upper end of the outer ring side. An axial sealing plate (13) is installed on the rotating core seat (12). An axial sealing assembly is provided at the outer end of the axial sealing plate (13). The axial sealing assembly includes a sealing spring ring (16). The sealing spring ring (16) is stacked in a ring and the ends are staggered from bottom to top with deformation grooves (17). A lead screw (14) is threaded to the upper end of the axial sealing plate (13). The lead screw (14) is fixedly connected to the top of the stator (2).

2. The high-pressure liquid phase medium sampling device according to claim 1, characterized in that, The valve seat (1) is connected to a quantitative ring (4), a sample flow path tube (5), and a waste liquid tube (6) via an interface cover (3).

3. The high-pressure liquid phase medium sampling device according to claim 2, characterized in that, The quantitative ring (4) is a hollow capillary channel with a fixed volume. The quantitative ring (4) is connected to two vertically corresponding interface caps (3) and is used for fixed-volume sampling of high-pressure liquid media.

4. The high-pressure liquid phase medium sampling device according to claim 3, characterized in that, The interface cap (3) is used to connect the sample flow path inlet, sample flow path outlet, quantitative loop (4) inlet, quantitative loop (4) outlet, manual injection port and waste liquid port respectively. The quantitative loop (4) inlet and quantitative loop (4) outlet are used to connect the quantitative loop (4) respectively. The waste liquid port is used to connect the waste liquid tube (6). The sample flow path inlet and sample flow path outlet are used to connect the sample flow path tube (5).

5. The high-pressure liquid phase medium sampling device according to claim 1, characterized in that, The stator (2) is provided with an indicator arrow (8) on the top for indicating the connection between the two arc-shaped flow channels (9) and the two sets of flow holes (10).

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