CN111282314A - Oil-water separation membrane and preparation method thereof - Google Patents
Oil-water separation membrane and preparation method thereof Download PDFInfo
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- CN111282314A CN111282314A CN202010189821.XA CN202010189821A CN111282314A CN 111282314 A CN111282314 A CN 111282314A CN 202010189821 A CN202010189821 A CN 202010189821A CN 111282314 A CN111282314 A CN 111282314A
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- 238000000926 separation method Methods 0.000 title claims abstract description 68
- 239000012528 membrane Substances 0.000 title claims abstract description 53
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 47
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 238000000576 coating method Methods 0.000 claims abstract description 34
- 239000011248 coating agent Substances 0.000 claims abstract description 30
- 239000002105 nanoparticle Substances 0.000 claims abstract description 30
- 230000002209 hydrophobic effect Effects 0.000 claims abstract description 23
- 239000002245 particle Substances 0.000 claims abstract description 21
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 claims abstract description 13
- 239000002904 solvent Substances 0.000 claims abstract description 7
- 238000004519 manufacturing process Methods 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 4
- 229910052751 metal Inorganic materials 0.000 claims description 4
- 239000002184 metal Substances 0.000 claims description 4
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 2
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 2
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 2
- 229910052801 chlorine Inorganic materials 0.000 claims description 2
- 239000000460 chlorine Substances 0.000 claims description 2
- 229910052731 fluorine Inorganic materials 0.000 claims description 2
- 239000011737 fluorine Substances 0.000 claims description 2
- 239000006260 foam Substances 0.000 claims description 2
- 125000001165 hydrophobic group Chemical group 0.000 claims description 2
- 229910052759 nickel Inorganic materials 0.000 claims description 2
- 229940089951 perfluorooctyl triethoxysilane Drugs 0.000 claims description 2
- 229920006254 polymer film Polymers 0.000 claims description 2
- 229910000077 silane Inorganic materials 0.000 claims description 2
- ZFUVZJADECZZMS-UHFFFAOYSA-N trichloro(3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,11,11,12,12,12-henicosafluorododecyl)silane Chemical compound FC(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)CC[Si](Cl)(Cl)Cl ZFUVZJADECZZMS-UHFFFAOYSA-N 0.000 claims description 2
- MLXDKRSDUJLNAB-UHFFFAOYSA-N triethoxy(3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10-heptadecafluorodecyl)silane Chemical compound CCO[Si](OCC)(OCC)CCC(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F MLXDKRSDUJLNAB-UHFFFAOYSA-N 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 13
- 239000000203 mixture Substances 0.000 abstract description 12
- 230000003075 superhydrophobic effect Effects 0.000 abstract description 3
- 230000003746 surface roughness Effects 0.000 abstract description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 24
- 239000004408 titanium dioxide Substances 0.000 description 12
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 10
- 229910052802 copper Inorganic materials 0.000 description 10
- 239000010949 copper Substances 0.000 description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- 238000001035 drying Methods 0.000 description 8
- 238000003756 stirring Methods 0.000 description 8
- 239000000758 substrate Substances 0.000 description 8
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 6
- 239000007788 liquid Substances 0.000 description 5
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 4
- 238000004140 cleaning Methods 0.000 description 4
- 238000000445 field-emission scanning electron microscopy Methods 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 239000004745 nonwoven fabric Substances 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- AVYKQOAMZCAHRG-UHFFFAOYSA-N triethoxy(3,3,4,4,5,5,6,6,7,7,8,8,8-tridecafluorooctyl)silane Chemical compound CCO[Si](OCC)(OCC)CCC(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F AVYKQOAMZCAHRG-UHFFFAOYSA-N 0.000 description 3
- 238000000861 blow drying Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000007602 hot air drying Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000007792 addition Methods 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000000703 high-speed centrifugation Methods 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- PISDRBMXQBSCIP-UHFFFAOYSA-N trichloro(3,3,4,4,5,5,6,6,7,7,8,8,8-tridecafluorooctyl)silane Chemical compound FC(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)CC[Si](Cl)(Cl)Cl PISDRBMXQBSCIP-UHFFFAOYSA-N 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
- B01D17/02—Separation of non-miscible liquids
- B01D17/0202—Separation of non-miscible liquids by ab- or adsorption
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- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
- Filtering Materials (AREA)
Abstract
The invention discloses an oil-water separation membrane and a preparation method thereof. According to the preparation method of the oil-water separation membrane, nano particles with different particle sizes and low surface energy fluoride are prepared into the hydrophobic coating by using a solvent, and then the hydrophobic coating is coated on the surface of the selected filter screen. According to the invention, the fluoride with low surface energy and the nano-particle mixed hydrophobic coating for improving the surface roughness are utilized to improve the hydrophobicity of the surface of the membrane, so that the surface of the membrane is super-hydrophobic, the holes of the filter screen can well improve the high pressure of the separation membrane material caused by bearing a water-oil mixture, and the oil-water separation efficiency can be improved, so that the bearing pressure and the separation efficiency of the membrane can be effectively improved.
Description
Technical Field
The invention relates to the technical field of separation membranes, in particular to an oil-water separation membrane and a preparation method thereof.
Background
The destruction of the ecological environment is a troublesome problem while the modern industrial development brings scientific and technological progress and the convenience of people's life. The industrial wastewater and various domestic sewage are discharged into the water body environment, oil-water separation is difficult to treat, and the problems of high adhesiveness, strong ecological environment pollution, incomplete separation and the like are always the key points of pollution prevention and control at present. In the traditional treatment means, physical separation modes such as high-speed centrifugation, physical sedimentation, solidification separation and the like have the problems of poor effect treatment, long consumed time, residual smell, occupation of a large amount of factory land area and the like, and a chemical separation method possibly has the problems of secondary pollution to the environment and the like. Based on this, a membrane separation method, which combines physical and chemical methods, has low production cost and high separation efficiency, and can meet the goals of environmental protection and treatment efficiency, has become a hot point of extensive research. The membrane separation method mainly utilizes different special wetting properties of the membrane surface to water and oil, such as a super-hydrophilic/super-oleophobic separation membrane, a super-hydrophobic/super-oleophilic separation membrane, a hydrophilic-hydrophobic reversible separation membrane and the like, and can prepare separation membrane materials with different requirements according to the actual treatment environment and the properties of treated liquid. However, the existing separation membrane material mainly has the problems that the membrane surface is difficult to bear the huge pressure of the mixed liquid of the water and the oil and the recycling rate of the separation membrane material, and the like, so people urgently hope to develop the membrane material for separating the oil and the water, which has high separation efficiency, can resist the liquid pressure, is economic and environment-friendly, and can be recycled continuously.
Disclosure of Invention
The invention aims to provide an oil-water separation membrane with high separation efficiency and high liquid bearing pressure and a preparation method thereof, aiming at the defects of the prior art.
According to the preparation method of the oil-water separation membrane, nano particles with different particle sizes and low surface energy fluoride are prepared into the hydrophobic coating by using a solvent, and then the hydrophobic coating is coated on the surface of the selected filter screen.
Preferably, the low surface energy fluoride comprises-CF3and/or-CF2A fluorine-containing hydrophobic group.
Preferably, the low surface energy fluoride comprises 1H,1H,2H, 2H-perfluorodecyltriethoxysilane, 1H,2H, 2H-perfluorooctyltriethoxysilane or 1H,1H,2H, 2H-perfluorooctyltriethoxysilane.
Preferably, the nanoparticles with different particle diameters comprise two nanoparticles with different particle diameter ranges, wherein one is the nanoparticle with the particle diameter of 20-100nm, the other is the nanoparticle with the particle diameter of 150-500nm, and the mass ratio of the small particle diameter to the large particle diameter is 1-10: 1.
Preferably, the solvent comprises absolute ethanol, isopropanol or water.
Preferably, the ratio of the nanoparticles to the low surface energy fluoride and solvent is 1g:1-5ml:95-99 ml.
Preferably, the filter screen comprises a metal mesh, a filter paper mesh, a nickel foam mesh or a polymer film mesh.
Preferably, the screen is a metal mesh and the low surface energy fluoride does not include a hydrophobic silane containing chlorine.
Preferably, the aperture of the filter screen is 0.05mm-1mm, and the pitch is 5-15 mm.
An oil-water separation membrane prepared by the preparation method.
According to the invention, the fluoride with low surface energy and the nano-particle mixed hydrophobic coating for improving the surface roughness are utilized to improve the hydrophobicity of the surface of the membrane, so that the surface of the membrane is super-hydrophobic, the holes of the filter screen can well improve the high pressure of the separation membrane material caused by bearing a water-oil mixture, and the oil-water separation efficiency can be improved, so that the bearing pressure and the separation efficiency of the membrane can be effectively improved.
Drawings
FIG. 1 is a graph showing the change of separation efficiency and separation time of 10 times of circulating oil-water separation on the surface of the oil-water separation membrane in example 1;
FIG. 2 is a graph showing the change in contact angle of the surface of the oil-water separation membrane of example 1 after 10 cycles of oil-water separation;
FIG. 3 is a FESEM photograph of the surface of the oil-water separation membrane of example 1;
fig. 4 is a partially enlarged FESEM view of fig. 3.
Detailed Description
The following are specific embodiments of the present invention and are further described with reference to the drawings, but the present invention is not limited to these embodiments.
The first embodiment is as follows:
(1) filter screen treatment
Selecting the type of a substrate material according to the actual oil-water separation condition, pricking a pinhole array with the diameter of 0.4mm, the depth of the pinhole array being 5mm and the distance (pitch) between the pinhole array and the pinhole array being 10mm on the surface of the filter paper, and obtaining the required filter paper mesh.
(2) Preparing a hydrophobic coating:
respectively weighing 0.1g of titanium dioxide nanoparticles (particle size range of 20-50nm) and 0.1g of titanium dioxide nanoparticles (particle size range of 160-200nm) and adding the titanium dioxide nanoparticles into a round-bottom flask containing 99ml of absolute ethyl alcohol, magnetically stirring the mixture at room temperature for 2 hours, adding 1ml of 1H,1H,2H, 2H-perfluoro octyl trichlorosilane, wrapping the round-bottom flask with tinfoil and keeping the round-bottom flask away from light, and continuously magnetically stirring the mixture at room temperature for 24 hours.
(3) Coating process treatment
Coating 1ml of hydrophobic coating on the surface of the filter paper net, uniformly mixing the residual hydrophobic coating after hot air drying for 5min, coating for the second time, repeatedly coating for 5 times, and drying by hot air to obtain the oil-water separation membrane taking the filter paper net as a base material.
Performance testing
The separation time and separation effect of the oil-water separation membrane prepared in example one, which was used to separate a mixture of water and dichloromethane in a circulating manner, are shown in fig. 1. It can be seen from fig. 1 that the water-oil separation ability of the separation membrane of this example is still good even after ten cycles.
Fig. 2 shows the change of the contact angle per cycle of the mixed liquid of water and dichloromethane separated by the oil-water separation membrane prepared in example one, and it can be seen from fig. 2 that the change of the contact angle is small and the water-oil separation capability of the separation membrane is still good.
FIG. 3 is a FESEM photograph of the surface of the oil-water separation membrane of example 1;
fig. 4 is a partially enlarged FESEM view of fig. 3.
It can be seen from fig. 3 and 4 that the surface of the oil-water separation membrane is rough.
After the surface of the nano-particles is coated, the size and the shape of pores can still keep the original good bearing pressure and separation efficiency, so that the influence of the nano-particles on the pores is very small, but the hydrophobic property of the whole separation membrane material can be improved, the separation efficiency is improved, the service life is prolonged, and the mutual synergistic effect of the nano-particles and the separation membrane is realized.
Example two:
(1) filter screen treatment
Selecting the type of a substrate material according to the actual oil-water separation condition, pricking pin holes with the diameter of 0.6mm and the depth of 8mm on the surface of the non-woven fabric (PET, 150g), and obtaining the required non-woven fabric filter screen, wherein the distance (pitch) between the pin holes is 8 mm.
(2) Preparing a hydrophobic coating:
respectively weighing 0.5g of titanium dioxide nanoparticles (particle size range of 20-50nm) and 0.1g of titanium dioxide nanoparticles (particle size range of 150-200nm) and adding the titanium dioxide nanoparticles into a round-bottom flask containing 95ml of absolute ethyl alcohol, magnetically stirring the mixture at room temperature for 2 hours, adding 1ml of 1H,1H,2H, 2H-perfluorododecyl trichlorosilane, wrapping the round-bottom flask with tinfoil and keeping the round-bottom flask away from light, and continuously magnetically stirring the mixture at room temperature for 24 hours.
(3) Coating process treatment
Coating 1ml of hydrophobic coating on the non-woven fabric filter screen, uniformly mixing the residual hydrophobic coating after hot air drying for 5min, coating for the second time, repeatedly coating for 5 times, and drying by hot air to obtain the oil-water separation membrane taking the non-woven fabric filter screen as a base material.
Example three:
(1) filter screen treatment
Ultrasonically cleaning a 10cm x 10cm copper sheet for 5min by using ionized water, drying the copper sheet by using nitrogen, cleaning the copper sheet by using absolute ethyl alcohol for 5min, and drying the copper sheet by using nitrogen for later use.
A needle hole with the needle diameter of 0.5mm can be pricked on the surface of the copper sheet by using the mechanical arm and the needle plate, the hole depth is 5mm, and the distance (pitch) between the needle hole and the needle hole is 10mm, so that the copper mesh is obtained.
(2) Preparing a hydrophobic coating:
respectively weighing 1g of titanium dioxide nanoparticles (the particle size range is 50-100nm) and 0.1g of titanium dioxide nanoparticles (the particle size range is 200-300nm) and adding the titanium dioxide nanoparticles into a round-bottom flask containing 99ml of absolute ethyl alcohol, magnetically stirring the mixture at room temperature for 2 hours, adding 1ml of 1H,1H,2H, 2H-perfluorooctyltriethoxysilane into the round-bottom flask, wrapping the round-bottom flask with tinfoil and keeping the round-bottom flask away from light, and continuously magnetically stirring the mixture at room temperature for 24 hours.
(3) Coating process treatment
Coating 1ml of hydrophobic coating on the surface of the copper mesh, after drying with hot air for 5min, uniformly mixing the residual hydrophobic coating, then coating for the second time, repeatedly coating for 5 times, and drying with hot air to obtain the oil-water separation membrane taking the copper mesh as a substrate material.
Example four:
(1) filter screen treatment
Ultrasonically cleaning a 10cm × 10cm copper net (100 meshes, with hole edge length of 0.15mm) with ionized water for 5min, blow-drying with nitrogen, cleaning with anhydrous ethanol for 5min, and blow-drying with nitrogen for later use.
(2) Preparing a hydrophobic coating:
respectively weighing 0.2g of titanium dioxide nanoparticles (the particle size range is 100-150nm) and 0.1g of titanium dioxide nanoparticles (the particle size range is 400-500nm) and adding the titanium dioxide nanoparticles into a round-bottom flask containing 95ml of water, magnetically stirring the mixture at room temperature for 2 hours, then adding 1ml of 1H,1H,2H, 2H-perfluorooctyltriethoxysilane into the mixture, wrapping the round-bottom flask with tinfoil and keeping the round-bottom flask away from light, and continuously magnetically stirring the mixture at room temperature for 24 hours.
(3) Coating process treatment
And soaking the substrate surface subjected to the substrate hole treatment in 10ml of hydrophobic coating for 5min, taking out the substrate surface, drying the substrate surface for 5min by hot air, uniformly mixing the rest hydrophobic coating, soaking for the second time, repeatedly carrying out the treatment for 5 times, and drying by hot air to obtain the oil-water separation membrane taking the copper mesh as the substrate material.
The above is not relevant and is applicable to the prior art.
While certain specific embodiments of the present invention have been described in detail by way of illustration, it will be understood by those skilled in the art that the foregoing is illustrative only and is not limiting of the scope of the invention, as various modifications or additions may be made to the specific embodiments described and substituted in a similar manner by those skilled in the art without departing from the scope of the invention as defined in the appending claims. It should be understood by those skilled in the art that any modifications, equivalents, improvements and the like made to the above embodiments in accordance with the technical spirit of the present invention are included in the scope of the present invention.
Claims (10)
1. A preparation method of an oil-water separation membrane is characterized by comprising the following steps: preparing nano particles with different particle sizes and low surface energy fluoride into a hydrophobic coating by using a solvent, and then coating the hydrophobic coating on the surface of the selected filter screen.
2. The method for producing an oil-water separation membrane according to claim 1, wherein: the low surface energy fluoride comprises-CF3and/or-CF2A fluorine-containing hydrophobic group.
3. The method for producing an oil-water separation membrane according to claim 2, wherein: the low surface energy fluoride comprises 1H,1H,2H, 2H-perfluorodecyl triethoxysilane, 1H,2H, 2H-perfluorooctyl triethoxysilane or 1H,1H,2H, 2H-perfluorododecyl trichlorosilane.
4. The method for producing an oil-water separation membrane according to claim 1, wherein: the nano-particles with different particle diameters comprise two nano-particles with different particle diameter ranges, wherein one nano-particle is 20-100nm, the other nano-particle is 150-500nm, and the mass ratio of the small particle diameter to the large particle diameter is 1-10: 1.
5. The method for producing an oil-water separation membrane according to claim 1, wherein: the solvent comprises absolute ethyl alcohol, isopropanol or water.
6. The method for producing an oil-water separation membrane according to claim 5, wherein: the ratio of the nanoparticles to the low surface energy fluoride and solvent is 1g:1-5ml:95-99 ml.
7. The method for producing an oil-water separation membrane according to claim 2, wherein: the filter screen comprises a metal mesh, a filter paper mesh, a foam nickel mesh or a polymer film mesh.
8. The method for producing an oil-water separation membrane according to claim 2, wherein: the screen is a metal mesh and the low surface energy fluoride does not include hydrophobic silane containing chlorine.
9. The method for producing an oil-water separation membrane as claimed in any one of claims 1 to 8, wherein: the aperture of the filter screen is 0.05mm-1mm, and the pitch is 5-15 mm.
10. An oil-water separation membrane produced by the production method according to any one of claims 1 to 9.
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| CN112691556A (en) * | 2020-12-31 | 2021-04-23 | 天津理工大学 | Method for preparing oil-water separation membrane by using melt-blown cloth layer of waste mask |
| CN115583738A (en) * | 2022-08-31 | 2023-01-10 | 浙江工业大学 | Oil-water-gas-solid four-phase separation device and separation method thereof |
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| CN104689602A (en) * | 2015-03-22 | 2015-06-10 | 河北工业大学 | Preparation method of inorganic substance coating oil-water separation mesh |
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- 2020-03-18 CN CN202010189821.XA patent/CN111282314A/en active Pending
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| CN104689602A (en) * | 2015-03-22 | 2015-06-10 | 河北工业大学 | Preparation method of inorganic substance coating oil-water separation mesh |
| CN109316778A (en) * | 2018-09-14 | 2019-02-12 | 浙江工业大学 | A kind of method that immersion coating polymer nano granules prepare super-hydrophobic copper mesh |
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| CN112691556A (en) * | 2020-12-31 | 2021-04-23 | 天津理工大学 | Method for preparing oil-water separation membrane by using melt-blown cloth layer of waste mask |
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Application publication date: 20200616 |