Microporous membrane for preparing high molecular microspheres and method for manufacturing the same

By using a protruding outlet end design in the microporous membrane, the tension and lateral shear force of the microdroplets are reduced, and the forward thrust is enhanced, thus solving the problem of microsphere inconsistency in the prior art and realizing the preparation of smaller and more uniform microspheres.

CN117656623BActive Publication Date: 2025-12-16ZHUZHOU SHUANGAN MICRO MEDICAL TECH CO LTD
View PDF 1 Cites 0 Cited by

Patent Information

Application Number
CN202311732717.0
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2023-12-15
Publication Date
2025-12-16
Estimated Expiration
2043-12-15

AI Technical Summary

Technical Problem

Existing methods for preparing polymer microspheres often result in poor microsphere size inconsistency, mainly due to the significant influence of interfacial tension of the membrane and shear force of the continuous liquid phase.

Method used

A novel microporous membrane is used, comprising a membrane body and a forming tube penetrating the membrane body. The outlet end of the forming tube protrudes from the membrane body. The raw material is output through the forming tube to form microdroplets, and the continuous phase liquid passes through along the thickness direction of the membrane body, reducing the tension of the microdroplets and providing a balanced pushing force to form microspheres with good consistency.

Benefits of technology

By reducing the tension and lateral shear force of the microdroplets and enhancing the positive thrust on the microdroplets, the stability and uniformity of the outer diameter of the microspheres are achieved, enabling the preparation of smaller and more uniform microspheres.

✦ Generated by Eureka AI based on patent content.

Smart Images

  • Figure CN117656623B_ABST
    Figure CN117656623B_ABST
Patent Text Reader

Abstract

The application discloses a microporous membrane for preparing high-molecular microspheres and a manufacturing method thereof. The microporous membrane comprises a membrane body and a plurality of forming tubes. The membrane body is provided with a plurality of micropores capable of allowing fluid to pass through the membrane body along the thickness direction of the membrane body. The forming tubes penetrate through the membrane body along the thickness direction of the membrane body, and the outlet ends of the forming tubes protrude from the membrane body. In application, raw materials are output at the outlet ends of the forming tubes and form microdroplets. Since the outlet ends of the forming tubes protrude from the membrane body, the tension on the microdroplets can be reduced, the microdroplets can more naturally form spherical shapes, and since the micropores of the membrane body can allow continuous phase liquid to pass through the membrane body along the thickness direction of the membrane body, the continuous phase liquid can push the microdroplets from the back side of the microdroplets, the force acting on the microdroplets is more balanced, and therefore, microspheres with good consistency can be output.
Need to check novelty before this filing date? Find Prior Art

Description

Technical Field

[0001] This invention relates to the field of polymer microsphere preparation technology, and in particular to a microporous membrane for preparing polymer microspheres and its manufacturing method. Background Technology

[0002] Currently, the main methods for preparing polymer microspheres include emulsification and solidification, microporous membrane emulsification, microfluidic preparation, coagulation, and spraying. In industrial production, emulsification and solidification, and the newest microporous membrane emulsification method, are the most commonly used. Figure 7 As shown, the microporous membrane emulsification method uses a straight-pore microporous membrane 910. Raw material 920 passes through the microporous membrane to form microdroplets. A continuous phase liquid 930, different from the raw material, is used to laterally flush the microdroplets, desorbing them. After solidification, the microdroplets form microspheres 940. During this process, the interfacial tension, pore density, and shear force of the continuous phase liquid have a significant impact on the formation of microspheres, resulting in varying sizes of polymer microspheres. Summary of the Invention

[0003] The present invention aims to at least solve one of the technical problems existing in the prior art. To this end, the present invention proposes a microporous membrane for preparing polymer microspheres, which can be used to prepare polymer microspheres with good consistency.

[0004] The present invention also proposes a method for manufacturing microporous membranes.

[0005] According to a first aspect of the present invention, a microporous membrane includes a membrane body and a plurality of forming tubes. The membrane body is provided with a plurality of micropores that allow fluid to pass through the membrane body along the thickness direction of the membrane body. The forming tubes penetrate the membrane body along the thickness direction of the membrane body, and the outlet end of the forming tubes protrudes from the membrane body.

[0006] The microporous membrane according to embodiments of the present invention has at least the following beneficial effects: In application, the raw material is output from the outlet end of the forming tube and forms microdroplets. Since the outlet end of the forming tube protrudes from the membrane body, the tension on the microdroplets can be reduced, and the microdroplets can form spherical shapes more naturally. Furthermore, since the micropores of the membrane body allow the continuous phase liquid to pass through the membrane body along the thickness direction of the membrane body, the continuous phase liquid can push the microdroplets from the rear side, resulting in a more balanced force on the microdroplets. Therefore, microspheres with better consistency can be output.

[0007] According to some embodiments of the present invention, the inlet end of the forming tube protrudes from the membrane body.

[0008] According to some embodiments of the present invention, the pore size of the micropore is 0.1 micrometers to 5 micrometers.

[0009] According to some embodiments of the present invention, the inner diameter of the molded tube is 20 micrometers to 100 micrometers.

[0010] According to some embodiments of the present application, the wall thickness of the forming tube is 20-100 microns.

[0011] According to some embodiments of the present application, the forming tube is a quartz tube.

[0012] According to some embodiments of the present application, the membrane body is a PVDF membrane or a PES membrane.

[0013] The method for manufacturing a microporous membrane according to the second aspect of the embodiments of the present application comprises the following steps:

[0014] Step 1, placing the forming tube in the mold to lay flat, first pouring the resin mixed solution in the mold;

[0015] Step 2, placing the mold in the displacement solution to displace the solvent in the resin mixed solution;

[0016] Step 3, taking out the mold to dry, obtaining a layered membrane with a set thickness;

[0017] Step 4, stacking and fixedly combining at least two of the layered membranes to form a multi-layer membrane;

[0018] Step 5, cutting the multi-layer membrane along the radial direction of the forming tube to obtain a membrane body with the forming tube embedded therein;

[0019] Step 6, spraying a solvent on the end face of the membrane body to dissolve the resin on the surface of the membrane body, so that the end portion of the forming tube is exposed, and the membrane body reaches a set thickness.

[0020] The method for manufacturing a microporous membrane according to the embodiments of the present application has at least the following beneficial effects: it can meet the manufacturing requirements of microporous membranes and is conducive to preparing microporous membranes with good consistency.

[0021] According to some embodiments of the present application, in step 1, the resin in the resin mixed solution is a PVDF resin or a PES resin.

[0022] According to some embodiments of the present application, in step 1, the resin mixed solution is a PVDF resin and DMF solvent mixture, and the solid content is 5%-15%.

[0023] According to some embodiments of the present application, in step 4, the at least two layered membranes are bonded by an adhesive and then hot-pressed to fuse to form the multi-layer membrane.

[0024] According to some embodiments of the present application, the adhesive is an acrylate adhesive, the hot-pressing temperature is 90-110°C, and the hot-pressing time is 5-10 seconds.

[0025] According to some embodiments of the present application, in step 2, the displacement liquid is water.

[0026] According to some embodiments of the present application, in step 3, the thickness of the layered film is 1±0.1 mm.

[0027] According to some embodiments of the present application, in step 4, 200±10 of the layered films are stacked and fixedly combined to form the multi-layered film.

[0028] According to some embodiments of the present application, in step 5, the multi-layered film is cut using a femtosecond laser.

[0029] According to some embodiments of the present application, step 6 comprises the following steps:

[0030] Step 6.1, spraying a set amount of solvent on the surface of the microporous film, then keeping at a temperature of 50±5°C for 5-10 seconds, and then rinsing the surface of the microporous film with a cleaning solution;

[0031] Step 6.2, repeating step 6.1 until the film body reaches a set thickness. BRIEF DESCRIPTION OF DRAWINGS

[0032] The above and / or additional aspects and advantages of the present application will become apparent and more readily appreciated from the following description of embodiments, taken in conjunction with the accompanying drawings in which:

[0033] Figure 1 Process diagram for preparing polymer microspheres from a microporous film according to embodiments of the present application;

[0034] Figure 2 Structure diagram of a layered film according to embodiments of the present application;

[0035] Figure 3 Structure diagram of a multi-layered film according to embodiments of the present application;

[0036] Figure 4 Structure diagram of a multi-layered film after cutting according to embodiments of the present application;

[0037] Figure 5 Structure diagram of a microporous film according to embodiments of the present application;

[0038] Figure 6 Microscopic diagram of a resin after displacement of a solvent in a resin mixed solution according to embodiments of the present application;

[0039] Figure 7 Process diagram for preparing polymer microspheres from a microporous film using a conventional emulsion method.

[0040] REFERENCE NUMERALS:

[0041] Membrane body 100, forming tube 200, layered membrane 300, multi-layer membrane 400, straight-hole microporous membrane 910, raw material 920, continuous phase liquid 930, microspheres 940. DETAILED DESCRIPTION

[0042] Embodiments of the present application are described below in detail, examples of which are shown in the drawings, wherein the same or similar reference signs represent the same or similar elements or elements having the same or similar functions throughout. The embodiments described below by referring to the drawings are exemplary, only for explaining the present application, and cannot be understood as limiting the present application.

[0043] In the description of the present application, it should be understood that the orientation description, such as the orientation or position relationship indicated by up, down, front, back, left, right, etc. is based on the orientation or position relationship shown in the drawings, only for the convenience of describing the present application and simplifying the description, and therefore cannot be understood as limiting the present application, which indicates or implies that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation.

[0044] In the description of the present application, if the first, second is described, it is only for the purpose of distinguishing technical features, and cannot be understood as indicating or implying the relative importance of the technical features indicated, or implicitly indicating the number of technical features indicated, or implicitly indicating the order of the technical features indicated.

[0045] In the description of the present application, unless otherwise explicitly limited, the words such as setting, installing, connecting, etc. should be broadly understood, and the person skilled in the art can reasonably determine the specific meaning of the above words in the present application in combination with the specific content of the technical solution.

[0046] In the related art, high molecular microspheres are prepared by microporous membrane emulsification method, such as Figure 7 As shown, the raw material 920 is arranged on one side of the straight-hole microporous membrane 910, and the continuous phase liquid 930 of different phase from the raw material is arranged on the other side of the straight-hole microporous membrane 910. The raw material 920 passes through the straight-hole microporous membrane 910 through the straight hole of the straight-hole microporous membrane 910, and forms microdroplets at the straight-hole outlet of the continuous phase liquid 930. The flow direction of the continuous phase liquid 930 is substantially perpendicular to the axial direction of the straight hole, so that the continuous phase liquid 930 laterally washes the microdroplets to detach the microdroplets, and the microdroplets are solidified to form microspheres 940. In this process, the interfacial tension of the membrane, the pore density and the lateral shear force of the continuous phase liquid have a great influence on the formation of the microspheres, resulting in different sizes of the high molecular microspheres and poor consistency.

[0047] The following refers to Figures 1 to 5 The microporous membrane for preparing high molecular microspheres and the manufacturing method thereof according to the embodiments of the present application are described.

[0048] As shown in Figure 1 ,Figure 5 As shown, the microporous membrane for preparing high-molecular microspheres according to the embodiments of the present application comprises a membrane body 100 and a plurality of forming tubes 200, the membrane body 100 is provided with a plurality of micropores capable of allowing fluid to pass through the membrane body 100 along the thickness direction of the membrane body 100; the forming tubes 200 penetrate the membrane body 100 along the thickness direction of the membrane body 100, and the outlet end of the forming tube 200 protrudes out of the membrane body 100; in application, the raw material 920 is output at the outlet end of the forming tube 200 and forms a microdroplet, since the outlet end of the forming tube 200 protrudes out of the membrane body 100, the tension on the microdroplet can be reduced, the microdroplet can form a spherical shape more naturally, and since the micropores of the membrane body 100 can allow the continuous phase liquid 930 to pass through the membrane body 100 along the thickness direction of the membrane body 100, the continuous phase liquid 930 can push the microdroplet from the back side (along the conveying direction of the raw material 920) of the microdroplet, and the force acting on the microdroplet is more balanced, so that microspheres 940 with good consistency can be output.

[0049] Specifically, in actual application, as shown in Figure 1 As shown, from left to right, they are a raw material area for feeding the raw material 920, a sandwich area for feeding the continuous phase liquid 930, a microporous membrane, and a forming area for forming microspheres, the raw material 920 passes through the membrane body 100 through the forming tube 200, is output at the outlet end of the forming tube 200, and forms a microdroplet, the continuous phase liquid 930 passes through the membrane body 100 through the micropores of the membrane body 100, passes through the microdroplet in the same direction as the conveying direction of the raw material 920, pushes the microdroplet from the back side of the microdroplet, and separates the microdroplet from the outlet end of the forming tube 200, and solidifies to form microspheres 940 in the forming area, since the microdroplet is subjected to smaller tension (reducing the interfacial tension of the membrane body 100), the lateral shear force of the continuous phase liquid 930 on the microdroplet is reduced, the forward pushing force on the microdroplet is increased, and the force is balanced (distributed around the microdroplet), so that the outer diameter of the microspheres 940 is stable and has good consistency.

[0050] Moreover, since the force exerted by the continuous phase liquid 930 on the microdroplet is more balanced, the forward pushing force of the continuous phase liquid 930 on the microdroplet can be set to be larger than the traditional lateral shear force, so that smaller and more uniform microspheres can be formed, and the production of smaller size microspheres can be met.

[0051] It can be conceived that in some embodiments of the present application, forming tubes 200 with different densities and different inner diameters can be configured as needed to meet different production requirements.

[0052] As shown in Figure 1 , Figure 5 In some embodiments of the present application, the inlet end of the forming tube 200 protrudes out of the membrane body 100 to separate the raw material 920 and the continuous phase liquid 930.

[0053] Specifically, as shown in Figure 1As shown, the inlet end of the forming tube 200 protrudes from the part of the membrane body 100 passing through the interlayer region for feeding the continuous phase liquid 930. In the specific embodiment, the raw material region is separated from the interlayer region (the raw material 920 and the continuous phase liquid 930) by a plate member, such as a metal plate, having a through hole matching the inlet end of the forming tube 200. The inlet end of the forming tube 200 is fixed after passing through the through hole, thereby separating the raw material 920 from the continuous phase liquid 930.

[0054] It is conceived that in some embodiments of the present application, the inlet end of the forming tube 200 can be arranged not to protrude from the membrane body 100, and the raw material 920 can be fed into the forming tube 200 by arranging an extension tube passing through the interlayer region and extending to the inlet end of the forming tube 200 in the raw material region.

[0055] According to some embodiments of the present application, the pore size of the micropores is 0.1-5 microns to meet the passing requirement of the continuous phase liquid 930.

[0056] Specifically, in the present application, the membrane body 100 is a porous structure to form the micropores and has good passing property, and the continuous phase liquid 930 is more uniformly distributed.

[0057] It is conceived that in some embodiments of the present application, the micropores can also be straight holes penetrating the membrane body 100.

[0058] The micropores can be straight holes or irregular holes, such as the porous structure of the membrane body 100.

[0059] According to some embodiments of the present application, the inner diameter of the forming tube 200 is 20-100 microns to meet the production requirement of the microparticles with a set diameter.

[0060] According to some embodiments of the present application, the wall thickness of the forming tube 200 is 20-100 microns to make the end of the forming tube 200 generate a suitable tension on the microparticles, so as not to be too large or too small.

[0061] According to some embodiments of the present application, the forming tube 200 is a quartz tube, and of course, in the specific implementation process, the forming tube 200 can also be a metal tube, etc., which is not described in detail herein.

[0062] According to some embodiments of the present application, the thickness of the membrane body 100 is 100±10 microns, which can better support the forming tube 200 and ensure the good passing property of the continuous phase liquid 930.

[0063] According to some embodiments of the present application, the membrane body 100 is a PVDF membrane or a PES membrane.

[0064] Specifically, PVDF membranes, or polyvinylidene fluoride membranes, are a commonly used solid-phase support in protein blotting. PVDF membranes are hydrophobic and can form a porous structure, meeting the requirement for continuous phase liquid flow at 930°C.

[0065] PES (polyethersulfone) membranes are membrane materials made by thermally bonding polyethersulfone ultrafine fibers together. They belong to the category of depth filtration membrane materials and meet the requirements for the passage of continuous phase liquid 930. PES membranes can be hydrophobic or hydrophilic, depending on their surface properties. In this embodiment, a hydrophilic PES microporous membrane is preferred to adapt to different and similar continuous phase liquids 930 (such as aqueous or oil phases) compared to the hydrophobic PVDF membrane.

[0066] According to some embodiments of the present invention, the continuous phase liquid 930 is determined according to the microsphere raw material. Generally speaking, if the raw material 920 is an aqueous phase, then an oil-phase continuous phase liquid 930 such as light paraffin oil is used. If the raw material 920 is an oil phase, then pure water is used for the continuous phase liquid 930.

[0067] According to an embodiment of the present invention, a production assembly for preparing polymer microspheres includes, from left to right, a raw material zone for feeding raw material 920, a sandwich zone for feeding continuous phase liquid 930, a microporous membrane as described in any of the above embodiments, and a forming zone for forming microspheres. The raw material 920 passes through the membrane body 100 via a forming tube 200 and exits at the outlet end of the forming tube 200 to form microdroplets. The continuous phase liquid 930 passes through the micropores of the membrane body 100 and passes through the microdroplets in the same direction as the conveying direction of the raw material 920. The microdroplets are pushed off the outlet end of the forming tube 200 from the rear side and solidify in the forming zone to form microspheres 940. Because the tension on the microdroplets is small (reducing the interfacial tension of the membrane body 100) and the lateral shear force of the continuous phase liquid 930 on the microdroplets is reduced, the positive thrust on the microdroplets is increased, and the forces are balanced (circular distribution of microdroplets), the outer diameter of the microspheres 940 is stable and the consistency is good.

[0068] like Figure 1 As shown, in some embodiments of the present invention, the inlet end of the forming tube 200 protrudes from the membrane body 100 to facilitate the separation of the raw material 920 from the continuous phase liquid 930.

[0069] Specifically, such as Figure 1As shown, the inlet end of the forming tube 200 protrudes from the part of the membrane body 100 passing through the interlayer region for feeding the continuous phase liquid 930. In the specific embodiment, the raw material region is separated from the interlayer region (the raw material 920 and the continuous phase liquid 930) by a plate member such as a metal plate provided with through holes matched with the inlet end of the forming tube 200. After the inlet end of the forming tube 200 is inserted into the through holes, the forming tube 200 is fixed, thereby separating the raw material 920 from the continuous phase liquid 930.

[0070] It is conceivable that in some embodiments of the present application, the raw material region and the interlayer region can be separated by a separator such as a plate member, a film material. The production assembly can be a whole cavity (formed by an outer shell), which is separated into a raw material region, an interlayer region, and a forming region by the separator and the microporous membrane respectively. The raw material region, the interlayer region, and the forming region are respectively provided with external structures for inputting or outputting corresponding substances.

[0071] Of course, in the specific implementation process, the raw material region, the interlayer region, and the forming region can also be independent cavities (formed by mutually independent outer shells), which will not be described in detail here.

[0072] The microporous membrane manufacturing method according to the embodiment of the present application comprises the following steps:

[0073] Step 1, place the forming tube 200 in the mold and first cast the resin mixed solution in the mold;

[0074] Step 2, place the mold in the displacement liquid to displace the solvent in the resin mixed solution with the displacement liquid;

[0075] Step 3, take out the mold and dry it to obtain a layered membrane 300 with a set thickness, and the layered membrane 300 is embedded with the forming tube 200;

[0076] Step 4, stack and fixedly combine at least two layered membranes 300 to form a multi-layered membrane 400;

[0077] Step 5, cut the multi-layered membrane 400 along the radial direction of the forming tube 200 to obtain a membrane body 100 embedded with the forming tube 200;

[0078] Step 6, spray the solvent on the end surface of the membrane body 100 to dissolve the resin on the surface of the membrane body 100, so that the end part of the forming tube 200 is exposed, and the membrane body 100 reaches the set thickness, and the microporous membrane is obtained.

[0079] Specifically, after the displacement liquid displaces the solvent in the resin mixed solution, a porous structure can be formed on the resin. After the resin is dried and solidified, the layered membrane 300 embedded with the forming tube 200 as shown can be formed. Figure 2 The plurality of layered membranes 300 are sequentially stacked and fixedly combined to form a multi-layered membrane 400 as shown. Figure 3The multi-layer film 400 is cut perpendicularly to the forming tube 200 (radial direction) to obtain a multi-layer film 400 as shown in FIG. 4B. Figure 4 The film body 100 with the forming tube 200 embedded is shown in FIG. 4C. Finally, the surface layer of the film body 100 is sprayed with a solvent to dissolve the surface layer of the film body 100, so that the end of the forming tube 200 is exposed, and a microporous membrane as shown in FIG. 4D is formed. Figure 5

[0080] According to some embodiments of the present application, in step 6, one side end surface of the film body 100 can be dissolved as needed to expose one end of the forming tube 200, or both side end surfaces of the film body 100 can be dissolved to expose both ends of the forming tube 200.

[0081] According to some embodiments of the present application, in step 1, the resin in the resin mixed solution is a PVDF resin or a PES resin.

[0082] Specifically, the PVDF resin can finally form a PVDF membrane, which is a kind of solid support commonly used in Western blotting. The PVDF membrane is hydrophobic and can form a porous structure to meet the passing requirements of the continuous phase liquid 930.

[0083] The PES resin can finally form a PES membrane, which is a kind of membrane material made of polyether sulfone ultra-fine fibers fused together, belonging to a deep filtration membrane material, meeting the passing requirements of the continuous phase liquid 930. The PES membrane can be hydrophobic or hydrophilic, depending on its surface properties. In this embodiment, a hydrophilic PES membrane microporous membrane is preferably used to adapt to different types of continuous phase liquids 930 (such as aqueous phase or oil phase) similar to the hydrophobic PVDF membrane.

[0084] In some embodiments of the present application, in step 1, the resin mixed solution is a mixture of PVDF resin and DMF solvent (N,N-dimethylformamide), and the solid content is 5%-15%, which can obtain a porous PVDF membrane to meet the passing requirements of the continuous phase liquid 930.

[0085] It is conceivable that in some embodiments of the present application, the resin mixed solution is a mixture of PES resin and NMP solvent (N-methyl pyrrolidone), and the ratio can also be set as needed, such as a solid content of 5%-15%.

[0086] According to some embodiments of the present application, in step 4, the at least two layered films 300 are bonded and heat-pressed to form a multi-layer film 400, so that the multi-layer film 400 has good structural strength.

[0087] ​According to some embodiments of the present invention, the adhesive is an acrylic adhesive. Of course, in specific implementations, the adhesive may also be a polyurethane adhesive, a polystyrene adhesive, etc., which will not be described in detail here.

[0088] According to some embodiments of the present invention, after the layered film 300 is bonded with an adhesive, it is pressed by a hot press at a temperature of 90°C-110°C and a pressing time of 5-10 seconds, which can give the multilayer film 400 good structural strength.

[0089] It is conceivable that, in some embodiments of the present invention, multiple layered films 300 may also be individually bonded by adhesive or individually by hot pressing, which will not be described in detail here.

[0090] According to some embodiments of the present invention, in step 2, the displacement liquid is water, which can replace the solvent in the resin mixture solution to form a porous resin structure.

[0091] Specifically, such as Figure 6 As shown, after solvent replacement, the resin can form a porous structure as shown in Figure 6. After the resin is cured, it forms micropores that allow the continuous phase liquid 930 to pass through.

[0092] According to some embodiments of the present invention, in step 3, the thickness of the layered membrane 300 is 1 ± 0.1 mm.

[0093] Specifically, the thickness of the layered membrane 300 can be set according to the outer diameter of the forming tube 200. In the specific implementation process, it can also be other thickness values, which will not be detailed here.

[0094] According to some embodiments of the present invention, in step 4, 200±10 sheets of layered film 300 are stacked and fixedly bonded to form a multilayer film 400.

[0095] In the specific implementation process, the number of layered membranes 300 in the multilayer membrane 400 is set according to actual production needs.

[0096] According to some embodiments of the present invention, in step 5, a femtosecond laser or a conventional laser is used to cut the multilayer film 400, and good cutting accuracy is achieved.

[0097] According to some embodiments of the present invention, step 6 includes the following steps: Step 6.1, spray a set amount of solvent onto the surface of the microporous membrane, then maintain it at a temperature of 50±5℃ for 5-10 seconds, and then rinse the surface of the microporous membrane with a cleaning solution; Step 6.2, repeat step 6.1 until the membrane body 100 reaches the set thickness, that is, repeatedly spray and clean the surface of the microporous membrane with solvent so that the end of the forming tube 200 is exposed and the membrane body 100 reaches the set thickness.

[0098] Specifically, in step 1, the resin mixed solution is a PVDF resin and DMF solvent mixture, and therefore in step 6, DMF solvent is used to spray and dissolve the PVDF resin on the surface of the microporous membrane.

[0099] Of course, in the actual implementation process, different solvents can be selected according to the actual needs (type of resin), such as when the resin mixed solution is a PES resin and NMP solvent, NMP solvent can be used to spray the surface of the microporous membrane in step 6.

[0100] It is conceivable that in some embodiments of the present application, the cleaning liquid is water, and of course, in the actual implementation process, the cleaning liquid can also be other liquids with low solubility to the resin, such as ethanol, etc.

[0101] Example 1

[0102] The microporous membrane manufacturing method comprises the following steps:

[0103] Step 1, place the forming tube 200 in the mold and lay it flat, first cast the resin mixed solution in the mold, the resin mixed solution is a PVDF resin and DMF solvent mixture, and the solid content is 10±1%;

[0104] Step 2, place the mold in water to displace the DMF solvent in the resin mixed solution with water;

[0105] Step 3, take out the mold and dry it to obtain a layered film 300 with a thickness of 1±0.1 mm, and the layered film 300 is embedded with the forming tube 200;

[0106] Step 4, bond 200 layered films 300 through an acrylate adhesive, and press them together through a hot press to form a multi-layer film 400, the hot pressing temperature is 100°C, and the hot pressing time is 8 seconds;

[0107] Step 5, cut the multi-layer film 400 along the radial direction of the forming tube 200 to obtain a film body 100 embedded with the forming tube 200;

[0108] Step 6, spray a certain amount of DMF solvent on the surface of the microporous membrane, then keep it at a temperature of 52°C for 7 seconds, and then rinse the surface of the microporous membrane with a cleaning liquid until the film body 100 reaches 100±1 microns and the two ends of the forming tube 200 are exposed.

[0109] A microporous membrane capable of preparing high molecular microspheres with good consistency can be obtained.

[0110] Example 2

[0111] The microporous membrane manufacturing method comprises the following steps:

[0112] Step 1, lay the forming tube 200 in the mold, first cast the resin mixed solution in the mold, the resin mixed solution is a mixed solution of PES resin and NMP solvent, and the solid content is 12±1%;

[0113] Step 2, place the mold in water to replace the NMP solvent in the resin mixed solution with water;

[0114] Step 3, take out the mold and dry it to obtain a layered film 300 with a thickness of 1±0.1mm, and the forming tube 200 is embedded in the layered film 300;

[0115] Step 4, bond 200 layered films 300 by polyurethane adhesive, and press them together by a hot press to form a multilayer film 400, the hot pressing temperature is 105℃, and the hot pressing time is 7 seconds;

[0116] Step 5, cut the multilayer film 400 along the radial direction of the forming tube 200 to obtain a film body 100 embedded with the forming tube 200;

[0117] Step 6, spray a certain amount of NMP solvent on the surface of the microporous membrane, then keep it at a temperature of 50℃ for 8 seconds, and then wash the surface of the microporous membrane with a cleaning solution until the film body 100 reaches 100±1 microns and the two ends of the forming tube 200 are exposed.

[0118] Thus, a microporous membrane capable of preparing high molecular microspheres with good consistency can be obtained.

[0119] Of course, the present application is not limited to the above-mentioned embodiments, and those skilled in the art can make equivalent modifications or replacements without departing from the spirit of the present application, and these equivalent modifications or replacements are all included in the scope defined by the claims of the present application.

Claims

1. A microporous membrane for preparing polymer microspheres, characterized in that, include: A membrane body (100) is provided with a plurality of micropores that allow fluid to pass through the membrane body (100) along the thickness direction of the membrane body (100); Multiple forming tubes (200) are provided, which penetrate the membrane body (100) along the thickness direction of the membrane body (100), and the outlet end of the forming tube (200) protrudes from the membrane body (100).

2. The microporous membrane for preparing polymer microspheres according to claim 1, characterized in that, The inlet end of the forming tube (200) protrudes from the membrane body (100).

3. The microporous membrane for preparing polymer microspheres according to claim 1, characterized in that, The pore size of the micropores is 0.1 micrometers to 5 micrometers.

4. The microporous membrane for preparing polymer microspheres according to claim 1, characterized in that, The inner diameter of the molded tube (200) is 20 micrometers to 100 micrometers, and the wall thickness of the molded tube (200) is 20 micrometers to 100 micrometers.

5. The microporous membrane for preparing polymer microspheres according to claim 1, characterized in that, The formed tube (200) is a quartz tube.

6. A method for manufacturing a microporous membrane as described in any one of claims 1 to 5, characterized in that, Includes the following steps: Step 1: Place the molding tube (200) into the mold and lay it flat. First, pour the resin mixture into the mold. Step 2: Place the mold into the displacement solution to allow the displacement solution to replace the solvent in the resin mixture solution; Step 3: Remove the mold and dry it to obtain a layered film of the set thickness (300). Step 4: Stack and fix at least two of the layered films (300) to form a multilayer film (400). Step 5: Cut the multilayer film (400) along the radial direction of the forming tube (200) to obtain a film body (100) embedded with the forming tube (200). Step 6: Spray solvent onto the end face of the membrane body (100) to dissolve the resin on the surface of the membrane body (100), so that the end of the molding tube (200) is exposed and the membrane body (100) reaches the set thickness.

7. The method for manufacturing a microporous membrane according to claim 6, characterized in that, In step 1, the resin in the resin mixture solution is PVDF resin or PES resin.

8. The method for manufacturing a microporous membrane according to claim 6, characterized in that, In step 1, the resin mixture is a mixture of PVDF resin and DMF solvent, with a solid content of 5%-15%.

9. The method for manufacturing a microporous membrane according to claim 6, characterized in that, In step 4, at least two of the layered films (300) are bonded together with an adhesive and then hot-pressed to form the multilayer film (400).

10. The method for manufacturing a microporous membrane according to claim 6, characterized in that, Step 6 includes the following steps: Step 6.1: Spray a set amount of solvent onto the surface of the microporous membrane, then keep it at a temperature of 50±5℃ for 5-10 seconds, and then rinse the surface of the microporous membrane with cleaning solution. Step 6.2: Repeat step 6.1 until the membrane body (100) reaches the set thickness.

Citation Information

Patent Citations

  • Microporous membrane for preparing polymer microspheres

    CN221417633U