CN115889145A - High-durability oil-water separation net and preparation method thereof - Google Patents
High-durability oil-water separation net and preparation method thereof Download PDFInfo
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- CN115889145A CN115889145A CN202211581987.1A CN202211581987A CN115889145A CN 115889145 A CN115889145 A CN 115889145A CN 202211581987 A CN202211581987 A CN 202211581987A CN 115889145 A CN115889145 A CN 115889145A
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- 238000000926 separation method Methods 0.000 title claims abstract description 62
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 60
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 238000000576 coating method Methods 0.000 claims abstract description 54
- 239000011248 coating agent Substances 0.000 claims abstract description 53
- 239000002105 nanoparticle Substances 0.000 claims abstract description 46
- 239000011347 resin Substances 0.000 claims abstract description 31
- 229920005989 resin Polymers 0.000 claims abstract description 31
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 30
- 229910021485 fumed silica Inorganic materials 0.000 claims abstract description 28
- 239000002131 composite material Substances 0.000 claims abstract description 27
- 238000000034 method Methods 0.000 claims abstract description 24
- 229910001220 stainless steel Inorganic materials 0.000 claims abstract description 17
- 239000010935 stainless steel Substances 0.000 claims abstract description 17
- 229920001661 Chitosan Polymers 0.000 claims abstract description 15
- 150000003242 quaternary ammonium salts Chemical class 0.000 claims abstract description 15
- 239000004925 Acrylic resin Substances 0.000 claims abstract description 13
- 229920000178 Acrylic resin Polymers 0.000 claims abstract description 13
- LWHQXUODFPPQTL-UHFFFAOYSA-M sodium;2,2,3,3,4,4,5,5,6,6,7,7,8,8,8-pentadecafluorooctanoate Chemical compound [Na+].[O-]C(=O)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F LWHQXUODFPPQTL-UHFFFAOYSA-M 0.000 claims abstract description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 24
- 239000000243 solution Substances 0.000 claims description 24
- 238000003756 stirring Methods 0.000 claims description 21
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- 239000006185 dispersion Substances 0.000 claims description 12
- 238000005507 spraying Methods 0.000 claims description 11
- 238000004519 manufacturing process Methods 0.000 claims description 10
- 239000000758 substrate Substances 0.000 claims description 9
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 235000019441 ethanol Nutrition 0.000 claims description 6
- SNGREZUHAYWORS-UHFFFAOYSA-N perfluorooctanoic acid Chemical compound OC(=O)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F SNGREZUHAYWORS-UHFFFAOYSA-N 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 239000010963 304 stainless steel Substances 0.000 claims description 4
- 229910000589 SAE 304 stainless steel Inorganic materials 0.000 claims description 4
- 239000003292 glue Substances 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 3
- -1 perfluorooctanoic acid sodium ethanol Chemical compound 0.000 claims description 3
- 230000004907 flux Effects 0.000 abstract description 5
- 239000003921 oil Substances 0.000 description 12
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 6
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000005299 abrasion Methods 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000001747 exhibiting effect Effects 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 210000002747 omentum Anatomy 0.000 description 2
- 238000005580 one pot reaction Methods 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 230000003746 surface roughness Effects 0.000 description 2
- 238000012876 topography Methods 0.000 description 2
- GFLJTEHFZZNCTR-UHFFFAOYSA-N 3-prop-2-enoyloxypropyl prop-2-enoate Chemical compound C=CC(=O)OCCCOC(=O)C=C GFLJTEHFZZNCTR-UHFFFAOYSA-N 0.000 description 1
- 239000004593 Epoxy Substances 0.000 description 1
- 241000282414 Homo sapiens Species 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229920006335 epoxy glue Polymers 0.000 description 1
- 239000002346 layers by function Substances 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 210000004379 membrane Anatomy 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000010705 motor oil Substances 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000000879 optical micrograph Methods 0.000 description 1
- 229920000371 poly(diallyldimethylammonium chloride) polymer Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 230000003075 superhydrophobic effect Effects 0.000 description 1
- 239000002352 surface water Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Images
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A20/00—Water conservation; Efficient water supply; Efficient water use
- Y02A20/20—Controlling water pollution; Waste water treatment
- Y02A20/204—Keeping clear the surface of open water from oil spills
Abstract
The embodiment of the disclosure discloses a preparation method of a high-durability oil-water separation net, wherein fumed silica nanoparticles are modified by adopting sodium perfluorooctanoate and chitosan quaternary ammonium salt, acrylic resin is introduced to prepare a coating based on a resin-coated nanoparticle composite structure, and the coating is sprayed on a stainless steel net, so that the oil-water separation net based on the resin-coated nanoparticle composite structure is prepared. The oil-water separation net prepared by adopting simple equipment and process has super-oleophobic/super-hydrophilic property and mechanical durability, and has higher separation efficiency and separation flux in a severe oil-water environment.
Description
Technical Field
The embodiment of the disclosure relates to the technical field of micro-nano manufacturing, in particular to a high-durability oil-water separation net based on a resin-coated nanoparticle composite structure and a preparation method thereof, which are simple in process and convenient to prepare.
Background
Frequent leakage of marine oil and discharge of oily wastewater can cause serious consequences to animals, human beings and the environment, and a mesh-membrane separation method is a research hotspot for the problem of oil-water separation due to low cost, high efficiency and stable performance. At present, most of super-hydrophobic/super-oleophylic net films for oil-water separation are easily polluted by oil in the separation process, so that the oil flux is reduced, and the materials need to be periodically cleaned. The super-hydrophilic/underwater super-oleophobic surface has excellent underwater oil resistance and can prevent the omentum from being polluted, but each pore of the underwater super-oleophobic surface needs to be pre-wetted by water and the oleophobic property of the omentum coating depends on the formation and maintenance of a surface water film, so that the application of the underwater super-oleophobic surface is limited. The coating surface with both super-oleophobic property and super-hydrophilic property in the air is an ideal material for realizing oil-water separation, and adding nano particles into modified liquid is a way for effectively improving the surface roughness and optimizing the oil-water separation capability of the coating.
Yang et al (Yang, zhang, xu, et al. Superhydrophic-superalphobic coatings [ J ]. J Phys Chem,2012,22 (7): 2834) obtained composite polymers with good oleophobic/hydrophilic properties by reacting SiO 2-doped PDDA with PFO, however, such coating surface adhesion materials are prone to peeling off, thereby reducing efficacy. Chen et al (Chen, dong, zhang, et al. A Novel Separation-based Superhydrophic/Superoleophilic Coating and Its Application in Oil-Water Separation: letter [ J ] Chemistry Letters,2020,49 (12)) propose spraying an epoxy glue solution on a substrate followed by multi-layer spraying of a Superoleophobic/Superhydrophilic Coating, the cured epoxy causing the Coating to adhere to the substrate surface, but this method only has a certain mechanical durability for the portion of the functional layer that is in close contact with the glue layer. Lu et al (Lu, li, miao, et al. Superhydrophic/super hydrophthalic shell powder coating as an aversive coating for bed oil/water and oil/oil separation [ J ]. Journal of Membrane Science,2021, 637) proposed spraying 3M binder onto the substrate surface, followed by repeated spraying of superoleophobic/superhydrophilic coating and 3M binder in that order, and finally finishing the preparation with the spraying of modified coating, which alternating spraying greatly improved the mechanical durability of the coating, but the preparation process was cumbersome.
Therefore, the inventor provides the high-durability oil-water separation net based on the resin-coated nanoparticle composite structure and the preparation method thereof, the oil-water separation net prepared by the method has super-oleophobic/super-hydrophilic property and mechanical durability, the manufacturing process is simple and convenient, and the cost is low.
Disclosure of Invention
The embodiment of the disclosure provides an oil-water separation net based on a resin-coated nanoparticle composite structure and a preparation method thereof, and the oil-water separation net has the advantages of simple and convenient process and low cost, and has super-oleophobic/super-hydrophilic property and mechanical durability.
According to an aspect of the present disclosure, a method for manufacturing a high durability oil-water separation net is provided, including: preparing a coating based on a resin-coated nanoparticle composite structure; spraying the prepared coating based on the resin-coated nano particle composite structure on a stainless steel substrate; and drying the coating to obtain the high-durability oil-water separation net with the coating based on the resin-coated nano particle composite structure.
Optionally, in the above method, the nanoparticles are fumed silica nanoparticles exhibiting a hydrophilicity with a specific surface area of 200m 2 /g。
Optionally, in the above method, the resin is a hydroxy acrylic resin.
Optionally, in the above method, the preparing the coating based on the resin-coated nanoparticle composite structure specifically includes: adding the fumed silica nano particles into absolute ethyl alcohol, and uniformly stirring to prepare fumed silica dispersion; adding perfluorooctanoic acid and sodium hydroxide into absolute ethyl alcohol, and uniformly stirring to prepare a perfluorooctanoic acid sodium ethanol solution; adding chitosan quaternary ammonium salt into deionized water, and uniformly stirring to prepare a chitosan quaternary ammonium salt water solution; adding the prepared sodium perfluorooctanoate ethanol solution and the prepared chitosan quaternary ammonium salt aqueous solution into the prepared fumed silica dispersion liquid under a stirring state, and reacting to prepare the super oleophobic/super hydrophilic coating; and adding the super oleophobic/super hydrophilic coating into an acrylic resin glue solution and uniformly stirring to prepare the coating with the resin-coated nano particle composite structure.
Alternatively, in the above method, the fumed silica particles are at a concentration of 0.013g/ml.
Optionally, in the above method, the mass ratio of the hydroxyacrylic resin to the fumed silica nanoparticles is 2.
Optionally, in the above method, the stainless steel substrate is a 304 stainless steel mesh of 100-400 mesh.
According to another aspect of the present disclosure, a high durability oil-water separation net prepared by the above preparation method is also proposed.
Compared with the prior art, the embodiment of the present disclosure has at least the following beneficial technical effects:
(1) The oil-water separation net prepared by adopting the gas-phase silica nanoparticle composite structure coated by the hydroxyl acrylic resin has super-oleophobic/super-hydrophilic property and mechanical durability, and has good practicability;
(2) The coating is prepared by adopting a one-pot method, the preparation related instruments and process are simple, the coating can be prepared at normal temperature, the reaction is mild, and the operation is convenient;
(3) The prepared separation net has good separation efficiency and separation flux in a complex and severe oil-water environment, and simultaneously keeps higher separation efficiency after multiple times of separation.
Drawings
FIG. 1 is a surface topography of a stainless steel mesh sample prepared by an embodiment of the present disclosure after oil and water are respectively added to the surface;
fig. 2 is an optical microscope image of a stainless steel mesh sample prepared by an embodiment of the present disclosure;
FIG. 3 is a Scanning Electron Microscope (SEM) image of a stainless steel mesh sample prepared according to an embodiment of the disclosure;
FIGS. 4A-4B are SEM images of the surface of a stainless steel mesh before and after 30 wear cycles, respectively;
FIG. 5 is a schematic flow chart of a method of making a highly durable oil water separation network as set forth in an embodiment of the present disclosure; and
fig. 6 is a schematic flow chart of the preparation method of the coating based on the resin-coated nanoparticle composite structure.
Detailed description of the preferred embodiment
According to the embodiment of the disclosure, a preparation method of a high-durability oil-water separation net based on a resin-coated nanoparticle composite structure is provided, which specifically comprises the following steps:
(1) Preparation of fumed silica dispersion: adding the fumed silica nano particles into absolute ethyl alcohol, and uniformly stirring;
(2) Preparation of the modified solution: adding perfluorooctanoic acid and sodium hydroxide into absolute ethyl alcohol, and reacting for a period of time; adding chitosan quaternary ammonium salt into deionized water, and uniformly stirring to obtain a chitosan quaternary ammonium salt aqueous solution;
(3) Adding a sodium perfluorooctanoate ethanol solution and a chitosan quaternary ammonium salt aqueous solution into the fumed silica dispersion under a stirring state, and reacting for a period of time to obtain a super oleophobic/super hydrophilic coating;
(4) Adding an acrylic resin glue solution into the super oleophobic/super hydrophilic coating;
(5) And spraying the obtained coating on a stainless steel net, and drying the coating to obtain the high-durability oil-water separation net based on the resin-coated nano particle composite structure.
In the preparation method, the 304 stainless steel mesh is sequentially and respectively put into solutions such as acetone, ethanol, deionized water and the like, and the stainless steel mesh is cleaned in an ultrasonic mode, so that the surface of the stainless steel mesh is clean;
in the above preparation method, the reaction temperature employed in all the reaction steps is room temperature;
in the above production method, the mass ratio of perfluorooctanoic acid to sodium hydroxide in step (2) is 10;
in the above preparation method, the acrylic resin in step (4) is a hydroxy acrylic resin, and is dissolved in ethyl acetate.
As an example, the above preparation method may include the steps of:
(1) 0.4g of fumed silica nanoparticles was added to 15mL of anhydrous ethanol, and magnetically stirred for 2 hours to obtain a fumed silica dispersion.
(2) 0.03g of chitosan quaternary ammonium salt is added into 2ml of deionized water, and the mixture is magnetically stirred for 30min to be completely dissolved to obtain a transparent and slightly viscous chitosan quaternary ammonium salt water solution which is marked as solution A.
(3) 0.05g of sodium hydroxide and 0.5g of perfluorooctanoic acid were added to 10ml of anhydrous ethanol, and the mixture was magnetically stirred for 1 hour to obtain a solution of sodium perfluorooctanoate in ethanol, which was designated as solution B.
(4) And (3) slowly adding the solution A prepared in the step (2) and the solution B prepared in the step (3) into the fumed silica dispersion under the condition of stirring, and magnetically stirring for 2 hours to prepare a modified nanoparticle dispersion.
(5) And (3) dissolving 0.8g of hydroxy acrylic resin in 2ml of ethyl acetate, slowly adding the solution into the modified nanoparticle dispersion liquid prepared in the step (4), and continuously stirring for 30min to prepare the coating.
(6) And (4) spraying the coating prepared in the step (5) on a stainless steel net to obtain the high-durability oil-water separation net based on the resin-coated nano particle composite structure.
FIG. 1 shows a topography of a sample of the oil-water separation net after oil and water are dropped on the surface, the oil drops are in a nearly spherical state on the coating, and the water is quickly wetted and completely spread on the surface, so that the prepared oil-water separation net is intuitively demonstrated to have excellent super-oleophobic/super-hydrophilic properties.
Tests show that the oil-water separation net prepared according to the scheme has the contact angle of engine oil on the surface of the oil-water separation net being 155 degrees and the contact angle of water on the surface of the oil-water separation net being 0 degree, the prepared oil-water separation net still keeps super-oleophobic/super-hydrophilic even after 30 times of abrasive paper abrasion circulation, and the oil-water separation net has the separation efficiency of more than 96 percent and the separation efficiency of 1.6 multiplied by 10 in mixed solution of oil and water (alkaline, acidic, neutral, cold and hot) 4 L/(m 2 H) separation throughput above, still with 96.33% separation efficiency after 20 separation cycles.
Fig. 2 shows an optical microscopic image of the prepared oil-water separation net sample, wherein the surface of the stainless steel net is completely covered by the fumed silica nano particles, so that the surface roughness is high, a certain mesh area is reserved, and the separation flux is high.
Fig. 3 shows a Scanning Electron Microscope (SEM) image of the oil-water separation mesh sample, and it can be seen that the micro-scale aggregates are overlapped with the nano-scale particles, the fumed silica has high porosity and specific surface area, and the micro-morphology of the micro-nano composite structure makes the stainless steel mesh have high super-wettability.
FIG. 4 shows SEM images of the surface of the oil-water separation net before and after 30 abrasion cycles, and the mechanical durability of the coating is tested, and the surface appearance of the coating before and after abrasion is not obviously changed due to the addition of the acrylic resin.
Fig. 5 shows a schematic flow chart of a method for preparing a high durability oil-water separation net according to an embodiment of the present disclosure. As shown in fig. 5, the preparation method may include: s505, preparing a coating based on a resin-coated nanoparticle composite structure; s510, spraying the prepared coating based on the resin-coated nano particle composite structure on a stainless steel substrate; and S515, drying the coating to obtain the high-durability oil-water separation net with the coating based on the resin-coated nanoparticle composite structure.
As an example, as shown in fig. 6, preparing a coating based on a resin-coated nanoparticle composite structure may include: s605, adding the fumed silica nano particles into absolute ethyl alcohol, and uniformly stirring to prepare fumed silica dispersion; s610, adding perfluorooctanoic acid and sodium hydroxide into absolute ethyl alcohol, and uniformly stirring to prepare a perfluorooctanoic acid sodium ethanol solution; s615, adding the chitosan quaternary ammonium salt into deionized water, and uniformly stirring to prepare a chitosan quaternary ammonium salt water solution; s620, adding the prepared sodium perfluorooctanoate ethanol solution and the chitosan quaternary ammonium salt aqueous solution into the prepared fumed silica dispersion liquid under a stirring state, and reacting to prepare a super-oleophobic/super-hydrophilic coating; and S625, adding the super oleophobic/super hydrophilic coating into an acrylic resin adhesive solution and uniformly stirring to prepare the coating based on the resin-coated nano particle composite structure.
Although in fig. 6, the various steps are shown in a certain order with respect to each other for ease of illustration, this is not meant to limit the principles of the present disclosure to the order described above. In practice, the steps may be adjusted in order according to actual needs, or performed in parallel. For example, steps S610, S615, and S620 may be performed simultaneously or the order may be reversed without departing from the principles of the present disclosure.
Optionally, in the above method, the nanoparticles are fumed silica nanoparticles exhibiting a hydrophilicity with a specific surface area of 200m 2 /g。
Optionally, in the above method, the resin is a hydroxy acrylic resin.
Alternatively, in the above method, the fumed silica particles are at a concentration of 0.013g/ml.
Optionally, in the above method, the mass ratio of the hydroxyacrylic resin to the fumed silica nanoparticles is 2.
Optionally, in the above method, the stainless steel substrate is a 304 stainless steel mesh of 100-400 mesh.
According to another aspect of the present disclosure, a high durability oil-water separation net prepared by the above preparation method is also proposed.
Compared with the prior art, the embodiment of the present disclosure has at least the following beneficial technical effects: the oil-water separation net prepared by coating the fumed silica nanoparticle composite structure with the hydroxyl acrylic resin has both super-oleophobic/super-hydrophilic property and mechanical durability, and has good practicability; the coating is prepared by adopting a one-pot method, the preparation related instruments and process are simple, the coating can be prepared at normal temperature, the reaction is mild, and the operation is convenient; the prepared separation net has good separation efficiency and separation flux in a complex and severe oil-water environment, and simultaneously keeps higher separation efficiency after multiple times of separation.
Claims (8)
1. A preparation method of a high-durability oil-water separation net comprises the following steps:
preparing a coating based on a resin-coated nanoparticle composite structure;
spraying the prepared coating based on the resin-coated nano particle composite structure on a stainless steel substrate; and
and after the coating is dried, obtaining the high-durability oil-water separation net with the coating based on the resin-coated nano particle composite structure.
2. The method according to claim 1, wherein the nanoparticles are fumed silica nanoparticles having a specific surface area of 200m 2 /g。
3. The production method according to claim 2, wherein the resin is a hydroxyacrylic resin.
4. The method of claim 3, wherein preparing a coating based on a resin-coated nanoparticle composite structure comprises:
adding the fumed silica nano particles into absolute ethyl alcohol, and uniformly stirring to prepare fumed silica dispersion;
adding perfluorooctanoic acid and sodium hydroxide into absolute ethyl alcohol, and uniformly stirring to prepare a perfluorooctanoic acid sodium ethanol solution;
adding chitosan quaternary ammonium salt into deionized water, and uniformly stirring to prepare a chitosan quaternary ammonium salt water solution;
adding the prepared sodium perfluorooctanoate ethanol solution and the chitosan quaternary ammonium salt aqueous solution into the prepared fumed silica dispersion liquid under the stirring state, and reacting to prepare the super-oleophobic/super-hydrophilic coating;
and adding the super oleophobic/super hydrophilic coating into an acrylic resin glue solution and uniformly stirring to prepare the coating with the resin-coated nano particle composite structure.
5. The production method according to claim 3, wherein the fumed silica particles are at a concentration of 0.013g/ml.
6. The production method according to claim 3, wherein the mass ratio of the hydroxyacrylic resin to the fumed silica nanoparticles is 2.
7. The production method according to any one of claims 1 to 6, wherein the stainless steel substrate is a 100-mesh 304 stainless steel mesh.
8. A highly durable oil-water separation net produced by the production method described in any one of claims 1 to 7.
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2022
- 2022-12-09 CN CN202211581987.1A patent/CN115889145A/en active Pending
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