Assembly filling method of suppressor and suppressor

Abstract

The application relates to the technical field of ion chromatography analysis, and discloses an assembly and filling method of an inhibitor and the inhibitor. The assembly and filling method of the inhibitor comprises the following steps: sequentially mounting an ion exchange membrane, an electrode transparent screen, a regeneration chamber and a reinforcing plate from inside to outside on both sides of a filling layer in sequence, and tightly fixing the whole assembly; installing a sieve plate and a conversion joint at the outlet end of the filling layer, wherein the diameter of micropores on the sieve plate is smaller than the diameter of filler particles; using a pump body to pump the prepared filler homogenate into the cavity of the filling layer at the inlet end of the filling layer, so that the filler homogenate completely fills the whole cavity of the filling layer, and the pressure of the filler homogenate in the cavity is kept for a set time; and installing a sieve plate and a conversion joint at the inlet end of the filling layer. The application makes the filler completely filled, uniformly distributed and tightly filled in the filling layer, improves the working performance of the inhibitor, makes the chromatographic peak shape more sharp during the use of the inhibitor, and effectively improves the accuracy and stability of chromatographic detection.

Description

Technical Field

[0001] This invention relates to the field of ion chromatography analysis technology, and in particular to an assembly and filling method for an inhibitor and an inhibitor. Background Technology

[0002] The basic structure of existing suppressors consists of electrodes, membranes, a filling layer, membranes, and electrodes arranged sequentially. The filling layer is the core functional area, primarily used for filling with filler material. The filling state of the filler directly affects the suppressor's performance. In existing technologies, the inlets and outlets of the filling layer are designed to be quite small. The filler is typically filled into the cavity of the filling layer by spreading. The specific filling and assembly process is as follows: first, the filler is manually and evenly spread inside the cavity of the filling layer; then, the membrane and electrodes are pressed firmly onto both sides of the filling layer; finally, the overall assembly of the suppressor is completed.

[0003] However, this filling and assembly method has the following obvious technical defects: the manually spread filler cannot completely fill the cavity of the filling layer, and the distribution of the filler in the filling layer is difficult to achieve an ideal uniform state. At the same time, the compactness of the filler is insufficient, and there is a loose problem. The above problems directly lead to the suppressor having poor chromatographic peak shape during actual use, which seriously affects the accuracy and stability of chromatographic detection.

[0004] Therefore, there is an urgent need for an assembly and filling method for the suppressor and a suppressor in order to solve the above-mentioned technical problems. Summary of the Invention

[0005] Based on the above, the purpose of this invention is to provide an assembly and filling method for an inhibitor and an inhibitor that enables the filler to be completely, evenly distributed, and tightly packed within the filling layer, thereby improving the working performance of the inhibitor and making the chromatographic peaks sharper during use, effectively enhancing the accuracy and stability of chromatographic detection.

[0006] To achieve this objective, the present invention adopts the following technical solution:

[0007] The assembly and filling method for the suppressor includes:

[0008] Ion exchange membranes are installed on both sides of the cavity of the filling layer;

[0009] Electrode meshes are installed in the fluid channels of the two regeneration chambers, and sealing rings are provided on the outer periphery of the two electrode meshes.

[0010] The two regeneration chambers are respectively installed on the outside of the two ion exchange membranes, so that the ion exchange membranes are pressed between the filling layer and the regeneration chambers;

[0011] Two reinforcing plates are respectively installed on the outside of the two regeneration chambers;

[0012] Fasteners are used to sequentially pass through each of the reinforcing plates and each of the regeneration chambers to press and fix the entire assembly, thus completing the initial assembly of the suppressor;

[0013] For the pre-assembled suppressor, a sieve plate and a conversion connector are installed at the outlet end of the filling layer, wherein the diameter of the micropores on the sieve plate is smaller than the diameter of the filler particles, and the filler particles are resin particles or silica particles.

[0014] At the inlet end of the filling layer, the prepared filler slurry is pressurized and pumped into the cavity of the filling layer by a pump body, so that the filler slurry completely fills the entire cavity of the filling layer, and the pressure of the filler slurry in the cavity is maintained for a set time, wherein the filler slurry is prepared by mixing the filler particles and the slurry solvent.

[0015] A sieve plate and a conversion joint are installed at the inlet end of the filling layer.

[0016] In some possible implementations, the filler particles are silica gel particles with a diameter ranging from 3 μm to 5 μm, and the diameter of the micropores on the sieve plate ranges from 0.5 μm to 2 μm.

[0017] In some possible implementations, the filling pressure when the filler slurry is pumped into the cavity of the filler layer is determined by the following formula:

[0018] P=kAL / d 2 ;

[0019] Wherein, P is the filling pressure of the filler slurry, in MPa; A is the cross-sectional area of ​​the cavity of the filling layer, in mm. 2 d is the particle size of the filler particles, in μm; L is the length of the filling layer, in mm; k is 0.00125 / π, in MPa / mm.

[0020] In some possible implementations, the relationship between the pore size D at the inlet end of the filling layer and the particle size d of the filler particles is: 25d≤D≤100d.

[0021] In some possible implementations, the packing slurry in the cavity is homogenized and pressurized for 10 minutes to 1 hour.

[0022] In some possible implementations, the ion exchange membrane has a pressure resistance range of 20 MPa to 40 MPa.

[0023] In some possible implementations, the regeneration chamber is made of PEEK, and the reinforcing plate is made of PEEK or steel.

[0024] The suppressor includes a filling layer, an ion exchange membrane, an electrode mesh, a regeneration chamber, a reinforcing plate, a sieve plate, and a conversion connector. The suppressor is manufactured using the assembly and filling method of the suppressor described in any of the above schemes.

[0025] The beneficial effects of this invention are:

[0026] This invention, by setting sieve plates at the inlet and outlet ends of the packing layer to block the outflow of packing particles, facilitates an increase in the size of the inlet and outlet of the packing layer, breaking the limitations of the original packing layer's small inlet and outlet on the packing process. This provides a structural basis for pump-in packing and successfully solves the problem of inefficient delivery of packing slurry into the packing layer. Furthermore, by adopting a pre-assembly and then filling process, the packing slurry is pumped into the packing layer under pressure, allowing it to completely fill the entire cavity of the packing layer under pressure, solving the problem of packing not being able to completely fill the cavity in the prior art. The pressurized pumping method ensures that the packing is evenly distributed within the packing layer under pressure, and the packing compactness is significantly improved, solving the problems of loose and uneven packing caused by the original sprinkle-type packing method. Because the packing is completely, evenly distributed, and compacted within the packing layer, the performance of the suppressor is directly improved, resulting in sharper chromatographic peaks during use, effectively improving the accuracy and stability of chromatographic detection. Attached Figure Description

[0027] Figure 1 This is a schematic diagram of the suppressor provided in an embodiment of the present invention;

[0028] Figure 2 This is an exploded view of the suppressor provided in an embodiment of the present invention;

[0029] Figure 3 This is a cross-sectional view of the suppressor provided in an embodiment of the present invention;

[0030] Figure 4 This is a flowchart of the assembly and filling method for the suppressor provided in the embodiments of the present invention;

[0031] Figure 5 This is a flowchart of the preliminary assembly process of the suppressor provided in the embodiment of the present invention.

[0032] In the picture:

[0033] 1. Filler layer; 11. Inlet end; 12. Outlet end; 13. Chamber; 2. Ion exchange membrane; 3. Electrode mesh; 4. Regeneration chamber; 41. Fluid channel; 5. Reinforcing plate; 6. Sieve plate; 7. Adapter; 8. Sealing ring; 9. Fastener; 10. Connector. Detailed Implementation

[0034] Embodiments of the present invention are described in detail below. Examples of these embodiments are shown in the accompanying drawings, wherein the same or similar reference numerals denote the same or similar components or components having the same or similar functions throughout. The embodiments described below with reference to the accompanying drawings are exemplary and intended to explain the present invention, and should not be construed as limiting the present invention.

[0035] In the description of this invention, unless otherwise explicitly specified and limited, the terms "connected," "linked," and "fixed" should be interpreted broadly. For example, they can refer to a fixed connection or a detachable connection; a mechanical connection or an electrical connection; a direct connection or an indirect connection through an intermediate medium; or the internal communication of two components or the interaction between two components. Those skilled in the art can understand the specific meaning of the above terms in this invention according to the specific circumstances.

[0036] In the description of this invention, unless otherwise expressly specified and limited, "above" or "below" the second feature can include direct contact between the first and second features, or contact between the first and second features through another feature between them. Furthermore, "above," "over," and "on top" of the second feature includes the first feature being directly above or diagonally above the second feature, or simply indicates that the first feature is at a higher horizontal level than the second feature. "Below," "below," and "under" the second feature includes the first feature being directly below or diagonally below the second feature, or simply indicates that the first feature is at a lower horizontal level than the second feature.

[0037] The technical solution of the present invention will be further described below with reference to the accompanying drawings and specific embodiments.

[0038] This invention provides an assembly and filling method for an inhibitor and an inhibitor itself, to solve the technical problems of existing inhibitors, such as the inability of the filler to fill the filling layer, uneven distribution of the filler, and low compaction, due to unreasonable design of the inlet and outlet of the filling layer and unreasonable filling process. This improves the peak shape of the chromatographic peaks when the inhibitor is in use, and enhances the working performance and chromatographic detection effect of the inhibitor.

[0039] like Figures 1 to 3As shown, the suppressor provided in this embodiment includes a filling layer 1, ion exchange membranes 2, electrode meshes 3, regeneration chambers 4, reinforcing plates 5, sieve plates 6, and conversion connectors 7. The filling layer 1 has an inlet end 11 and an outlet end 12 at both ends along its length. A cavity 13 is etched or milled inside the filling layer 1, penetrating the filling layer 1 along its thickness direction, and communicating with the inlet end 11 and the outlet end 12 respectively. Two ion exchange membranes 2 are respectively attached to both sides of the filling layer 1 along its thickness direction, completely covering the outside of the cavity 13. Thus, the two ion exchange membranes 2 and the cavity 13 together form a closed cavity for filling the packing material and purging the eluent. Each of the two regeneration chambers 4 is provided with a fluid channel 41 for purging the regeneration solution. Two electrode meshes 3 are respectively installed in the two fluid channels 41, and each electrode mesh 3 has a sealing ring 8 on its outer periphery to seal the flow path and prevent cross-flow and leakage between the flow paths. Here, it is important to note that the contour of the sealing ring 8 should match the contour of the electrode mesh 3 to ensure good sealing performance. After assembling the electrode mesh 3 and the sealing ring 8, the two regeneration chambers 4 are respectively pressed onto the outer sides of the two ion exchange membranes 2, thereby pressing the ion exchange membranes 2 tightly between the filling layer 1 and the regeneration chambers 4, effectively preventing deformation and bulging of the ion exchange membranes 2. Two reinforcing plates 5 are respectively set on the outer sides of the two regeneration chambers 4 to enhance the rigidity and deformation resistance of the overall structure. Fasteners 9 are inserted sequentially from one side into one reinforcing plate 5, one regeneration chamber 4, another regeneration chamber 4, and another reinforcing plate 5, thereby pressing and fixing the entire assembly. Specifically, the fasteners 9 are fastening bolts. Furthermore, the suppressor is also provided with several connectors 10.

[0040] Furthermore, in this embodiment, the inlet end 11 and outlet end 12 of the cavity 13 are enlarged, and a sieve plate 6 and a conversion connector 7 are installed at both the inlet end 11 and outlet end 12. The sieve plate 6 is provided with multiple micropores, the diameter of which is smaller than the diameter of the packing particles, thereby preventing the packing material inside the cavity 13 from leaking outward. This embodiment enlarges the originally small inlet and outlet of the existing packing layer, which can adapt to the pump-in packing filling process and provides a channel guarantee for the smooth delivery of the packing slurry; at the same time, the enlarged inlet and outlet also reduces the processing difficulty of the inlet and outlet channels of the cavity 13. It should be noted that in this embodiment, the inlet end 11 and outlet end 12 are only named for convenience of description. The two have the same structure and there is no special limitation. In actual use, only one of them needs to be selected as the inlet and the other as the outlet.

[0041] Optionally, in this embodiment, the filling layer 1, the regeneration chamber 4, and the reinforcing plate 5 are all made of rigid materials. Specifically, the rigid material can be one of engineering plastics, polyetheretherketone (PEEK), a metal with an inert coating, or a special alloy. For example, the regeneration chamber 4 is made of PEEK, and the reinforcing plate 5 is made of PEEK or stainless steel, which effectively improves its structural strength and protects the ion exchange membrane 2 from deformation. Optionally, the electrode mesh 3 in this embodiment is a porous conductive mesh made of platinum-plated titanium mesh, stainless steel mesh, or precious metal materials, which makes the electrode mesh 3 highly corrosion-resistant, highly catalytically active, highly conductive, and structurally stable. Optionally, the sieve plate 6 is made of polyethylene, polytetrafluoroethylene, PEEK, or stainless steel to ensure its corrosion resistance and chemical stability.

[0042] like Figure 4 As shown, the assembly and filling method for the suppressor provided in this embodiment includes the following steps:

[0043] S1. Install the ion exchange membrane 2, electrode mesh 3, regeneration chamber 4 and reinforcing plate 5 on both sides of the filling layer 1 in order from the inside to the outside, and press and fix the entire assembly to complete the initial assembly of the suppressor.

[0044] Specifically, such as Figure 5 As shown, the initial assembly of the suppressor includes the following sub-steps:

[0045] S11. Ion exchange membranes 2 are attached to both sides of the cavity 13 of the filling layer 1.

[0046] S12. Install electrode mesh 3 in the fluid channels 41 of the two regeneration chambers 4 respectively, and set sealing rings 8 on the outer periphery of the two electrode mesh 3.

[0047] S13. Install the two regeneration chambers 4 on the outside of the two ion exchange membranes 2 respectively, so that the ion exchange membranes 2 are pressed between the filling layer 1 and the regeneration chambers 4 to form a laminated structure with a stable interface.

[0048] In this step, since both sides of the ion exchange membrane 2 are rigidly constrained, irregular bulging or separation from the channel wall is avoided, thus ensuring the consistency of the channel geometry and minimizing and stabilizing the dead volume.

[0049] S14. Install the two reinforcing plates 5 on the outside of the two regeneration chambers 4 respectively;

[0050] S15. Fasteners 9 are used to sequentially pass through each reinforcing plate 5 and each regeneration chamber 4 to press and fix the entire assembly, thereby forming a strong and sealed whole.

[0051] S2. For the initially assembled suppressor, install a sieve plate 6 and a conversion joint 7 at the outlet end 12 of the filling layer 1, wherein the diameter of the micropores on the sieve plate 6 is smaller than the diameter of the filler particles.

[0052] In this step, by installing a sieve plate 6 and a conversion connector 7 at the outlet end 12 of the filling layer 1, while keeping the inlet end 11 open, a sealed cavity with single-end liquid inlet can be formed in the filling layer 1.

[0053] S3. At the inlet end 11 of the filling layer 1, the prepared filler slurry is pressurized and pumped into the cavity 13 of the filling layer 1 using a pump body, so that the filler slurry completely fills the entire cavity 13 of the filling layer 1 without leaving any gaps.

[0054] It should be noted that during the filling and homogenization process, the sieve plate 6 at the outlet end 12 of the filling layer 1 can block the filler particles, preventing them from being flushed out by the flowing phase. Meanwhile, the high-pressure, high-speed liquid flow can expel the gas from the cavity 13, facilitating the filling. Thus, this embodiment achieves complete filling of the entire cavity 13 with the filler slurry through a single-end pumping method.

[0055] S4. After filling is completed, install the sieve plate 6 and the conversion joint 7 at the inlet end 11 of the filling layer 1 to prevent the filling material from leaking from the inlet end 11.

[0056] The assembly and filling method of the suppressor provided in this embodiment, by setting sieve plates 6 at the inlet end 11 and outlet end 12 of the filling layer 1 to block the outflow of filler particles, facilitates the increase of the size of the inlet and outlet of the filling layer 1, breaks the limitation of the filling process on the small inlet and outlet of the original filling layer 1, provides a structural basis for pump-in filling, and successfully solves the problem that the filler slurry cannot be efficiently delivered into the filling layer 1; by adopting the process of assembly before filling, the filler slurry is pumped into the filling layer 1 by the pump body, so that the filler slurry can completely fill the entire cavity 13 of the filling layer 1 under pressure, solving the problem that the filler cannot fill the cavity of the filling layer in the prior art; and the pressurized pumping method makes the filler uniformly distributed in the filling layer 1 under pressure, and the compactness of the filler is greatly improved, solving the problem of loose and uneven distribution of the filler caused by the original sprinkle-type filling method; since the filler is completely filled, uniformly distributed and compacted in the filling layer 1, the working performance of the suppressor is directly improved, making the peak shape of the chromatographic peaks sharper during the use of the suppressor, effectively improving the accuracy and stability of chromatographic detection.

[0057] Optionally, in this embodiment, the filler particles are resin particles. The filler slurry is specifically prepared by mixing the filler particles with a slurry solvent. Specifically, the slurry solvent can be pure water, a carbon tetrachloride / methanol mixture, or a tetrabromoethane / methanol mixture, etc. This configuration avoids the phenomenon of filler particle agglomeration during the filling and operation process. Optionally, in this embodiment, the filler particles are silica gel particles, which have good mechanical strength, can withstand the high-pressure impact during filling and use without easily breaking, and the particle size uniformity of silica gel particles is good, which is beneficial to improving the compactness of the filling. Furthermore, the diameter of the silica gel particles ranges from 3μm to 5μm, for example, 3μm, 3.2μm, 3.5μm, 3.8μm, 4μm, 4.2μm, 4.5μm, 4.8μm, 5μm, etc.; the diameter of the micropores on the sieve plate 6 ranges from 0.5μm to 2μm, for example, 0.5μm, 0.8μm, 1μm, 1.2μm, 1.5μm, 1.8μm, 2μm, etc. In this embodiment, by reducing the particle size of the silica gel particles, the detection accuracy can be greatly improved; and by reducing the diameter of the micropores on the sieve plate 6, the leakage of silica gel particles from the micropores can be effectively prevented, ensuring that the silica gel particles are completely trapped in the cavity 13 of the filling layer 1.

[0058] Optionally, the filling pressure when the filler slurry is pumped into the cavity 13 of the filling layer 1 is determined by the following formula:

[0059] P=kAL / d 2 ;

[0060] Where P is the filling pressure of the filler slurry, in MPa; A is the cross-sectional area of ​​cavity 13 of filling layer 1, in mm. 2 ; d is the particle size (i.e., diameter) of the filler particles, in μm; L is the length of filler layer 1, in mm; k is 0.00125 / π, in MPa / mm.

[0061] In this embodiment, the filling pressure P of the filler slurry is calculated using the above formula. Under this filling pressure, the filler slurry can be injected quickly and tightly into the cavity 13 of the filling layer 1. Specifically, in this embodiment, the cavity 13 is streamlined and spindle-shaped, with a wide middle section and smooth tapering at both ends. For this cavity 13 structure, A in the above formula is the cross-sectional area of ​​the middle section of the cavity 13.

[0062] Because the filler particles are small in size, in order to improve the compactness of the filler particles, in this embodiment, after the filler slurry fills the cavity 13 of the filling layer 1, it is necessary to maintain pressure. Therefore, after step S3 and before step S4, the following is also included: setting a time for maintaining pressure on the filler slurry in the cavity 13. Specifically, the pressure maintaining time can be set to 10 minutes to 1 hour, for example, 10 minutes, 20 minutes, 30 minutes, 40 minutes, 50 minutes, 1 hour, etc.; the pressure maintaining pressure is set to 20% to 100% of the filling pressure, for example, 20%, 30%, 40%, 50%, 60%, 70%, 80%, 90%, 100% of the filling pressure, etc. In this embodiment, by first pressing the filler slurry at a certain pressure at a uniform speed, and then maintaining pressure on the filler slurry in the cavity 13, the compactness of the filler is effectively improved, so that the filler can press tightly against the ion exchange membrane 2 after filling, thereby improving the detection effect of the suppressor.

[0063] Optionally, in this embodiment, the relationship between the pore size D of the inlet end 11 of the filling layer 1 and the particle size d of the packing particles is: 25d ≤ D ≤ 100d. For example, the pore size D of the inlet end 11 of the filling layer 1 can be 25 times, 30 times, 40 times, 50 times, 60 times, 70 times, 80 times, 90 times, 100 times, etc., the particle size d of the packing particles. If the pore size D of the inlet end 11 is too large, it will easily increase the dead volume; if the pore size D of the inlet end 11 is too small, it will cause the filling pressure to be too high, which may cause bulging of the ion exchange membrane 2. This embodiment effectively reduces the dead volume and keeps the filling pressure within a suitable range by reasonably designing the pore size D of the inlet end 11. Preferably, in this embodiment, D = 50d.

[0064] Furthermore, in this embodiment, the pressure resistance range of the ion exchange membrane 2 is 20MPa-40MPa, for example, it can be 20MPa, 25MPa, 30MPa, 35MPa, 40MPa, etc. Exemplarily, the ion exchange membrane 2 can be a perfluorosulfonic acid composite membrane, an ETFE (ethylene-tetrafluoroethylene copolymer) composite membrane, etc. This gives the ion exchange membrane 2 good strength, enabling it to maintain structural integrity during the filling process and use, and preventing the membrane surface from being damaged by pressure.

[0065] Obviously, the above embodiments of the present invention are merely examples for clearly illustrating the present invention, and are not intended to limit the implementation of the present invention. Those skilled in the art can make other variations or modifications based on the above description. It is neither necessary nor possible to exhaustively describe all embodiments here. Any modifications, equivalent substitutions, and improvements made within the spirit and principles of the present invention should be included within the scope of protection of the claims of the present invention.

Claims

1. A method for assembling and filling a suppressor, characterized in that, include: Ion exchange membranes (2) are installed on both sides of the cavity (13) of the filling layer (1); Electrode meshes (3) are installed in the fluid channels (41) of the two regeneration chambers (4), and sealing rings (8) are provided on the outer periphery of the two electrode meshes (3). The two regeneration chambers (4) are respectively installed on the outside of the two ion exchange membranes (2), so that the ion exchange membranes (2) are pressed between the filling layer (1) and the regeneration chambers (4); Two reinforcing plates (5) are respectively installed on the outside of the two regeneration chambers (4); Fasteners (9) are used to sequentially pass through each of the reinforcing plates (5) and each of the regeneration chambers (4) to press and fix the entire assembly, thus completing the initial assembly of the suppressor; For the pre-assembled suppressor, a sieve plate (6) and a conversion connector (7) are installed at the outlet end (12) of the filling layer (1), wherein the diameter of the micropores on the sieve plate (6) is smaller than the diameter of the filler particles, and the filler particles are resin particles or silica particles. At the inlet end (11) of the filling layer (1), the prepared filler slurry is pressurized and pumped into the cavity (13) of the filling layer (1) by a pump body, so that the filler slurry completely fills the entire cavity (13) of the filling layer (1), and the filler slurry in the cavity (13) is pressurized for a set time, wherein the filler slurry is prepared by mixing the filler particles with a slurry solvent; A sieve plate (6) and a conversion joint (7) are installed at the inlet end (11) of the filling layer (1).

2. The assembly and filling method for the suppressor according to claim 1, characterized in that, The filler particles are silica gel particles with a diameter range of 3μm-5μm, and the diameter range of the micropores on the sieve plate (6) is 0.5μm-2μm.

3. The assembly and filling method for the suppressor according to claim 1, characterized in that, The filling pressure when the filler slurry is pumped into the cavity (13) of the filling layer (1) is determined by the following formula: P=kAL / d 2 ; Wherein, P is the filling pressure of the filler slurry, in MPa; A is the cross-sectional area of ​​the cavity (13) of the filling layer (1), in mm. 2 ; d is the particle size of the filler particles, in μm; L is the length of the filling layer (1), in mm; k is 0.00125 / π, in MPa / mm.

4. The assembly and filling method for the suppressor according to claim 1, characterized in that, The relationship between the aperture D of the inlet end (11) of the filling layer (1) and the particle size d of the filler particles is: 25d≤D≤100d.

5. The assembly and filling method for the suppressor according to claim 1, characterized in that, The time for homogenizing and pressurizing the filler in the cavity (13) is 10 minutes to 1 hour.

6. The assembly and filling method for the suppressor according to claim 1, characterized in that, The pressure range of the ion exchange membrane (2) is 20MPa-40MPa.

7. A suppressor, comprising a filling layer (1), an ion exchange membrane (2), an electrode mesh (3), a regeneration chamber (4), a reinforcing plate (5), a sieve plate (6), and a conversion connector (7), characterized in that, The suppressor is manufactured using the assembly and filling method for suppressors as described in any one of claims 1-6.

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