CN101085417A - Hydrophilic and compaction resistant polyvinylidene fluoride ultrafilter membrane and preparation method thereof - Google Patents
Hydrophilic and compaction resistant polyvinylidene fluoride ultrafilter membrane and preparation method thereof Download PDFInfo
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- CN101085417A CN101085417A CN 200710072442 CN200710072442A CN101085417A CN 101085417 A CN101085417 A CN 101085417A CN 200710072442 CN200710072442 CN 200710072442 CN 200710072442 A CN200710072442 A CN 200710072442A CN 101085417 A CN101085417 A CN 101085417A
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Abstract
The invention relates to the making of polyvinylidene fluoride hyperfilteration film with hydrophilicity and resistance to pressure. It solves the poor hydrophilicity and resistance to pressure feature of polyvinylidene fluoride hyperfilteration film. It is made of polyvinylidene fluoride, ferric salt and acetic acid dimethylamide in weight percentages. The making comprises the making of casting film oil, debubbled casting film oil, liquid film, and final product film. It reduces resistance to water by 40-65%, increased hydrophilicity by 30-50% and resistance to pressure 65-85%.
Description
Technical field
The present invention relates to a kind of polyvinylidene fluoride (PVDF) ultrafiltration membrane and preparation method thereof.
Background technology
Kynoar (PVDF) is a kind of novel fluorocarbon thermoplastic plastics, vitrification point is-39 ℃, brittle temperature is below-62 ℃, crystalline melt point is 180 ℃, heat decomposition temperature is more than 316 ℃, long-term serviceability temperature scope is-50～150 ℃, still can keep good intensity under uniform temperature and pressurized; Its another outstanding advantage is to have excellent uvioresistant and a weatherability, and its film is in outdoor placement one, the be full of cracks that also do not become fragile in 20 years; In addition, the Kynoar chemical stability is good, at room temperature not by corrosion such as acid, alkali, strong oxidizers, only is dissolved in dimethyl formamide, dimethylacetylamide, some intensive polar solvents such as dimethyl sulfoxide (DMSO).Because it has above-mentioned plurality of advantages, and can curtain coating form permeability film preferably, unlike polytetrafluoroethylene (PTFE), polypropylene owing to there is not suitable solvent to prepare with methods such as fusion drawn, caused the equipment complexity, drawbacks such as preparation condition harshness, therefore PVDF becomes a kind of desirable separation membrane material, applicable to fields such as chemical industry, water treatment, electronics, weaving, food, biochemistry.But because polyvinylidene fluoride surface can be low, by its milipore filter of preparing very strong hydrophobicity is arranged, the one side hydrophobicity was unfavorable for that water passes through film when this film was used to water treatment, and the water flux that shows as film is low, needs higher mistake film pressure; A series of hydrophobicity organic pollutions such as protein in the water in the absorption of film surface, produce gel layer easily on the other hand, thereby polluted membrane reduces the water flux of film; In addition, the loose structure on the film section is under high mistake film pressure effect, and being easy to can be by densification, and this also will make the water flux of film further descend, and these performances of polyvinylidene fluoride (PVDF) ultrafiltration membrane have all influenced its application in engineering of water treatment.
Summary of the invention
The objective of the invention is problem poor for the hydrophily that solves existing polyvinylidene fluoride (PVDF) ultrafiltration membrane, the close property of resistance to compression difference, and proposed a kind of hydrophily and compaction resistant polyvinylidene fluoride ultrafilter membrane and preparation method thereof.A kind of hydrophily and compaction resistant polyvinylidene fluoride ultrafilter membrane according to percentage by weight by 14～25% Kynoar, make in the molysite of iron 0.2～3% and 72～85.8% dimethylacetylamide.The preparation method of a kind of hydrophily and compaction resistant polyvinylidene fluoride ultrafilter membrane realizes according to following steps: one, according to percentage by weight with 14～25% Kynoar, fully mix in the molysite of iron 0.2～3% and 72～85.8% dimethylacetylamide, obtain casting solution; Two, casting solution is put into beaker, under 25～80 ℃ temperature, the beaker that casting solution is housed carried out water-bath heating 3～10 hours and with 300～1000 rev/mins speed casting solution is stirred simultaneously, the hermetically sealed can of then casting solution being put in the hermetically sealed can and will be equipped with casting solution is put into 30～80 ℃ water standing and defoaming 15～72 hours, obtains the casting solution after the deaeration; Three, the casting solution after the deaeration is spread to the liquid film of 20～200 micron thickness with knifing machine on the film support in system, will stick together that the system of liquid film film support is arranged is that 5～35 ℃, wet-bulb temperature are that 5～35 ℃, relative humidity are to leave standstill evaporation 5～280 seconds under 25～95% the condition at dry-bulb temperature; Four, will stick together and have the system of liquid film film support to invade in 5～45 ℃ the distilled water to soak 5～10 minutes, this moment, liquid film came off from the system film support, the distilled water of liquid film being put into room temperature soaked 3～4 days, change first water in per 8～9 hours during immersion, promptly obtain a kind of hydrophily and compaction resistant polyvinylidene fluoride ultrafilter membrane.The molysite additive of selecting for use among the present invention can improve the water flux of film significantly and the cutoff performance of film too be reduced, can produce suitable macroporous structure on the film section to reduce the resistance of water when the film, the existing polyvinylidene fluoride (PVDF) ultrafiltration membrane of the resistance ratios of water has been reduced by 40～65%; Polyvinylidene fluoride (PVDF) ultrafiltration membrane surface among the present invention has generated FeOOH, this hydroaropic substance and film matrix bond are together, can not lose with current, thereby the hydrophily of film is significantly improved, and the hydrophily of the polyvinylidene fluoride (PVDF) ultrafiltration membrane among the present invention has improved 30～50% than existing polyvinylidene fluoride (PVDF) ultrafiltration membrane; Generate the common particle of forming of the oxide by Kynoar and iron that is evenly distributed on the film section of the polyvinylidene fluoride (PVDF) ultrafiltration membrane of the present invention's preparation, thereby the densification that milipore filter is showed under pressure is subjected to effective inhibition, show the close property of tangible resistance to compression, the close property of the resistance to compression of the polyvinylidene fluoride (PVDF) ultrafiltration membrane among the present invention has improved 65～85% than existing polyvinylidene fluoride (PVDF) ultrafiltration membrane; Preparation method among the present invention is simple and easy to do.
Description of drawings
Fig. 1 is the polyvinylidene fluoride (PVDF) ultrafiltration membrane profile scanning Electronic Speculum figure that the specific embodiment 31 is prepared, and Fig. 2 is the electron-microscope scanning figure of sponge structure on the polyvinylidene fluoride (PVDF) ultrafiltration membrane film section prepared of the specific embodiment 31.
The specific embodiment
The specific embodiment one: in the present embodiment a kind of hydrophily and compaction resistant polyvinylidene fluoride ultrafilter membrane according to percentage by weight by 14～25% Kynoar, make in the molysite of iron 0.2～3% and 72～85.8% dimethylacetylamide.
The specific embodiment two: the difference of the present embodiment and the specific embodiment one be a kind of hydrophily and compaction resistant polyvinylidene fluoride ultrafilter membrane according to percentage by weight by 16～23% Kynoar, make in the molysite of iron 0.5～2.6% and 74.4～83.5% dimethylacetylamide.
The specific embodiment three: the difference of the present embodiment and the specific embodiment one be a kind of hydrophily and compaction resistant polyvinylidene fluoride ultrafilter membrane according to percentage by weight by 18～21% Kynoar, make in the molysite of iron 0.7～2.3% and 76.7～81.3% dimethylacetylamide.
The specific embodiment four: the difference of the present embodiment and the specific embodiment one be a kind of hydrophily and compaction resistant polyvinylidene fluoride ultrafilter membrane according to percentage by weight by 19% Kynoar, make in the molysite and 80% dimethylacetylamide of iron 1%.
The specific embodiment five: the difference of the present embodiment and the specific embodiment one be a kind of hydrophily and compaction resistant polyvinylidene fluoride ultrafilter membrane according to percentage by weight by 15% Kynoar, make in the molysite and 83.8% dimethylacetylamide of iron 1.2%.
The specific embodiment six: the difference of the present embodiment and the specific embodiment one be a kind of hydrophily and compaction resistant polyvinylidene fluoride ultrafilter membrane according to percentage by weight by 18% Kynoar, make in the molysite and 80.5% dimethylacetylamide of iron 1.5%.
The specific embodiment seven: the difference of the present embodiment and the specific embodiment one be a kind of hydrophily and compaction resistant polyvinylidene fluoride ultrafilter membrane according to percentage by weight by 21% Kynoar, make in the molysite and 76.3% dimethylacetylamide of iron 2.7%.
The specific embodiment eight: the difference of the present embodiment and the specific embodiment one be a kind of hydrophily and compaction resistant polyvinylidene fluoride ultrafilter membrane according to percentage by weight by 1 5% Kynoar, make in the molysite and 84.7% dimethylacetylamide of iron 0.3%.
The specific embodiment nine: the difference of the present embodiment and the specific embodiment one is that molysite is frerrous chloride, contains in frerrous chloride, the ferric trichloride of the crystallization water, the ferric trichloride that contains the crystallization water, ferrous sulfate, ferric sulfate, ferrous nitrate or the ferric nitrate one or more, when molysite is two or more, between the molysite any mass ratio.Other composition is identical with the specific embodiment one.
The specific embodiment ten: the preparation method of a kind of hydrophily and compaction resistant polyvinylidene fluoride ultrafilter membrane realizes according to following steps in the present embodiment: one, according to percentage by weight with 14～25% Kynoar, fully mix in the molysite of iron 0.2～3% and 72～85.8% dimethylacetylamide, obtain casting solution; Two, casting solution is put into beaker, under 25～80 ℃ temperature, the beaker that casting solution is housed carried out water-bath heating 3～10 hours and with 300～1000 rev/mins speed casting solution is stirred simultaneously, the hermetically sealed can of then casting solution being put in the hermetically sealed can and will be equipped with casting solution is put into 30～80 ℃ water standing and defoaming 15～72 hours, obtains the casting solution after the deaeration; Three, the casting solution after the deaeration is spread to the liquid film of 20～200 micron thickness with knifing machine on the film support in system, will stick together that the system of liquid film film support is arranged is that 5～35 ℃, wet-bulb temperature are that 5～35 ℃, relative humidity are to leave standstill evaporation 5～280 seconds under 25～95% the condition at dry-bulb temperature; Four, will stick together and have the system of liquid film film support to invade in 5～45 ℃ the distilled water to soak 5～10 minutes, this moment, liquid film came off from the system film support, the distilled water of liquid film being put into room temperature soaked 3～4 days, change first water in per 8～9 hours during immersion, promptly obtain a kind of hydrophily and compaction resistant polyvinylidene fluoride ultrafilter membrane.
A kind of hydrophily and the compaction resistant polyvinylidene fluoride ultrafilter membrane of present embodiment preparation have reduced by 20～30% to the existing polyvinylidene fluoride (PVDF) ultrafiltration membrane of the resistance ratios of water; Polyvinylidene fluoride (PVDF) ultrafiltration membrane surface among the present invention has generated FeOOH, this hydroaropic substance and film matrix bond are together, can not lose with current, thereby the hydrophily of film is significantly improved, and the hydrophily of the polyvinylidene fluoride (PVDF) ultrafiltration membrane among the present invention has improved 60～80% than existing polyvinylidene fluoride (PVDF) ultrafiltration membrane; Generate the common particle of forming of the oxide by Kynoar and iron that is evenly distributed on the film section of the polyvinylidene fluoride (PVDF) ultrafiltration membrane of the present invention's preparation, thereby the densification that milipore filter is showed under pressure is subjected to effective inhibition, show the close property of tangible resistance to compression, the close property of the resistance to compression of the polyvinylidene fluoride (PVDF) ultrafiltration membrane among the present invention has improved 40～70% than existing polyvinylidene fluoride (PVDF) ultrafiltration membrane; Preparation method among the present invention is simple and easy to do.
The specific embodiment 11: present embodiment and the difference of the specific embodiment ten are in the step 1 according to percentage by weight with 16～23% Kynoar, fully mix in the molysite of iron 0.5～2.6% and 74.4～83.5% dimethylacetylamide.Other step is identical with the specific embodiment ten.
The specific embodiment 12: present embodiment and the difference of the specific embodiment ten are in the step 1 according to percentage by weight with 18～21% Kynoar, fully mix in the molysite of iron 0.7～2.3% and 76.7～81.3% dimethylacetylamide.Other step is identical with the specific embodiment ten.
The specific embodiment 13: present embodiment and the difference of the specific embodiment ten are in the step 1 according to percentage by weight with 19% Kynoar, fully mix in the molysite and 80% dimethylacetylamide of iron 1%.Other step is identical with the specific embodiment ten.
The specific embodiment 14: the difference of the present embodiment and the specific embodiment ten is in the step 2 that under 35～70 ℃ temperature the beaker that casting solution is housed carried out the water-bath heating 5～8 hours and with 400～800 rev/mins speed casting solution is stirred simultaneously.Other step is identical with the specific embodiment ten.
The specific embodiment 15: the difference of the present embodiment and the specific embodiment ten is in the step 2 that under 40～60 ℃ temperature the beaker that casting solution is housed carried out the water-bath heating 5.5～7.5 hours and with 500～700 rev/mins speed casting solution is stirred simultaneously.Other step is identical with the specific embodiment ten.
The specific embodiment 16: the difference of the present embodiment and the specific embodiment ten is in the step 2 that under 55 ℃ temperature the beaker that casting solution is housed carried out the water-bath heating 7 hours and with 600 rev/mins speed casting solution is stirred simultaneously.Other step is identical with the specific embodiment ten.
The specific embodiment 17: the difference of the present embodiment and the specific embodiment ten is in the step 2 that under 63 ℃ temperature the beaker that casting solution is housed carried out the water-bath heating 6.8 hours and with 550 rev/mins speed casting solution is stirred simultaneously.Other step is identical with the specific embodiment ten.
The specific embodiment 18: the hermetically sealed can that the difference of the present embodiment and the specific embodiment ten is in the step 2 to put into casting solution in the hermetically sealed can and casting solution will be housed is put into 35～70 ℃ water standing and defoaming 18～62 hours.Other step is identical with the specific embodiment ten.
The specific embodiment 19: the hermetically sealed can that the difference of the present embodiment and the specific embodiment ten is in the step 2 to put into casting solution in the hermetically sealed can and casting solution will be housed is put into 40～65 ℃ water standing and defoaming 20～58 hours.Other step is identical with the specific embodiment ten.
The specific embodiment 20: the hermetically sealed can that the difference of the present embodiment and the specific embodiment ten is in the step 2 to put into casting solution in the hermetically sealed can and casting solution will be housed is put into 55 ℃ water standing and defoaming 50 hours.Other step is identical with the specific embodiment ten.
The specific embodiment 21: the hermetically sealed can that the difference of the present embodiment and the specific embodiment ten is in the step 2 to put into casting solution in the hermetically sealed can and casting solution will be housed is put into 75 ℃ water standing and defoaming 30 hours.Other step is identical with the specific embodiment ten.
The specific embodiment 22: the difference of the present embodiment and the specific embodiment ten is in the step 3 casting solution after the deaeration to be spread on the system film support with knifing machine the liquid film of 40～180 micron thickness.Other step is identical with the specific embodiment ten.
The specific embodiment 23: the difference of the present embodiment and the specific embodiment ten is in the step 3 casting solution after the deaeration to be spread on the system film support with knifing machine the liquid film of 80～120 micron thickness.Other step is identical with the specific embodiment ten.
The specific embodiment 24: the difference of the present embodiment and the specific embodiment ten is will stick together in the step 3 that the system of liquid film film support is arranged is that 10～30 ℃, wet-bulb temperature are that 10～30 ℃, relative humidity are to leave standstill evaporation 20～230 seconds under 80～90% the condition at dry-bulb temperature.Other step is identical with the specific embodiment ten.
The specific embodiment 25: the difference of the present embodiment and the specific embodiment ten is will stick together in the step 3 that the system of liquid film film support is arranged is that 13～26 ℃, wet-bulb temperature are that 14～26 ℃, relative humidity are to leave standstill evaporation 50～220 seconds under 82～88% the condition at dry-bulb temperature.Other step is identical with the specific embodiment ten.
The specific embodiment 26: the difference of the present embodiment and the specific embodiment ten is will stick together in the step 3 that the system of liquid film film support is arranged is that 15～22 ℃, wet-bulb temperature are that 16～22 ℃, relative humidity are to leave standstill evaporation 70～200 seconds under 84～87% the condition at dry-bulb temperature.Other step is identical with the specific embodiment ten.
The specific embodiment 27: the difference of the present embodiment and the specific embodiment ten is will stick together in the step 3 that the system of liquid film film support is arranged is that 18 ℃, wet-bulb temperature are that 18 ℃, relative humidity are to leave standstill evaporation 150 seconds under 86% the condition at dry-bulb temperature.Other step is identical with the specific embodiment ten.
The specific embodiment 28: the difference of the present embodiment and the specific embodiment ten is will stick together in the step 4 in the distilled water that 10～35 ℃ of the system of liquid film film support intrusions are arranged and soaked 6～8 minutes.Other step is identical with the specific embodiment ten.
The specific embodiment 29: the difference of the present embodiment and the specific embodiment ten is will stick together in the step 4 in the distilled water that 12～32 ℃ of the system of liquid film film support intrusions are arranged and soaked 6.5～7.8 minutes.Other step is identical with the specific embodiment ten.
The specific embodiment 30: the difference of the present embodiment and the specific embodiment ten is will stick together in the step 4 in the distilled water that 20 ℃ of the system of liquid film film support intrusions are arranged and soaked 7 minutes.Other step is identical with the specific embodiment ten.
The specific embodiment 31: present embodiment realizes by following steps: one, according to percentage by weight with 18% Kynoar, fully mix in the frerrous chloride that contains 4 moles of crystallizations water of iron 3% and 79% dimethylacetylamide, obtain casting solution; Two, casting solution is put into beaker, under 60 ℃ temperature, the beaker that casting solution is housed carried out water-bath heating 4 hours and with 1000 rev/mins speed casting solution is stirred simultaneously, the hermetically sealed can of then casting solution being put in the hermetically sealed can and will be equipped with casting solution is put into 50 ℃ water standing and defoaming 48 hours, obtains the casting solution after the deaeration; Three, the casting solution after the deaeration is spread to the liquid film of 200 micron thickness with knifing machine on the film support in system, will stick together that the system of liquid film film support is arranged is that 19.5 ℃, wet-bulb temperature are that 13.5 ℃, relative humidity are to leave standstill evaporation 20 seconds under 45% the condition at dry-bulb temperature; Four, will stick together and have the system of liquid film film support to invade in 25 ℃ the distilled water to soak 10 minutes, this moment, liquid film came off from the system film support, the distilled water of liquid film being put into room temperature soaked 3 days, change first water in per 8 hours during immersion, promptly obtain a kind of hydrophily and compaction resistant polyvinylidene fluoride ultrafilter membrane.
A kind of hydrophily of present embodiment preparation and the film section electron-microscope scanning figure of compaction resistant polyvinylidene fluoride ultrafilter membrane can produce suitable macroporous structure on the film section, the resistance when helping reducing water by film as shown in Figure 1; The electron-microscope scanning figure of sponge structure finds the even structure of film as shown in Figure 2 on a kind of hydrophily of present embodiment preparation and the film section of compaction resistant polyvinylidene fluoride ultrafilter membrane, and the sponge structure prosperity helps the raising of the close property of resistance to compression of film.
Claims (10)
1, a kind of hydrophily and compaction resistant polyvinylidene fluoride ultrafilter membrane, it is characterized in that a kind of hydrophily and compaction resistant polyvinylidene fluoride ultrafilter membrane according to percentage by weight by 14～25% Kynoar, make in the molysite of iron 0.2～3% and 72～85.8% dimethylacetylamide.
2, a kind of hydrophily according to claim 1 and compaction resistant polyvinylidene fluoride ultrafilter membrane, it is characterized in that a kind of hydrophily and compaction resistant polyvinylidene fluoride ultrafilter membrane according to percentage by weight by 16～23% Kynoar, make in the molysite of iron 0.5～2.6% and 74.4～83.5% dimethylacetylamide.
3, a kind of hydrophily according to claim 1 and compaction resistant polyvinylidene fluoride ultrafilter membrane, it is characterized in that a kind of hydrophily and compaction resistant polyvinylidene fluoride ultrafilter membrane according to percentage by weight by 18～21% Kynoar, make in the molysite of iron 0.7～2.3% and 76.7～81.3% dimethylacetylamide.
4, a kind of hydrophily according to claim 1 and compaction resistant polyvinylidene fluoride ultrafilter membrane, it is characterized in that a kind of hydrophily and compaction resistant polyvinylidene fluoride ultrafilter membrane according to percentage by weight by 19% Kynoar, make in the molysite and 80% dimethylacetylamide of iron 1%.
5, a kind of hydrophily according to claim 1 and compaction resistant polyvinylidene fluoride ultrafilter membrane, it is characterized in that molysite is frerrous chloride, contains in frerrous chloride, the ferric trichloride of the crystallization water, the ferric trichloride that contains the crystallization water, ferrous sulfate, ferric sulfate, ferrous nitrate or the ferric nitrate one or more, when molysite is two or more, between the molysite any mass ratio.
6, the preparation method of a kind of hydrophily and compaction resistant polyvinylidene fluoride ultrafilter membrane, the preparation method who it is characterized in that a kind of hydrophily and compaction resistant polyvinylidene fluoride ultrafilter membrane realizes according to following steps: one, according to percentage by weight with 14～25% Kynoar, fully mix in the molysite of iron 0.2～3% and 72～85.8% dimethylacetylamide, obtain casting solution; Two, casting solution is put into beaker, under 25～80 ℃ temperature, the beaker that casting solution is housed carried out water-bath heating 3～10 hours and with 300～1000 rev/mins speed casting solution is stirred simultaneously, the hermetically sealed can of then casting solution being put in the hermetically sealed can and will be equipped with casting solution is put into 30～80 ℃ water standing and defoaming 15～72 hours, obtains the casting solution after the deaeration; Three, the casting solution after the deaeration is spread to the liquid film of 20～200 micron thickness with knifing machine on the film support in system, will stick together that the system of liquid film film support is arranged is that 5～35 ℃, wet-bulb temperature are that 5～35 ℃, relative humidity are to leave standstill evaporation 5～280 seconds under 25～95% the condition at dry-bulb temperature; Four, will stick together and have the system of liquid film film support to invade in 5～45 ℃ the distilled water to soak 5～10 minutes, this moment, liquid film came off from the system film support, the distilled water of liquid film being put into room temperature soaked 3～4 days, change first water in per 8～9 hours during immersion, promptly obtain a kind of hydrophily and compaction resistant polyvinylidene fluoride ultrafilter membrane.
7, the preparation method of a kind of hydrophily according to claim 6 and compaction resistant polyvinylidene fluoride ultrafilter membrane is characterized in that in the step 1 according to percentage by weight with 16～23% Kynoar, fully mix in the molysite of iron 0.5～2.6% and 74.4～83.5% dimethylacetylamide.
8, the preparation method of a kind of hydrophily according to claim 6 and compaction resistant polyvinylidene fluoride ultrafilter membrane is characterized in that in the step 2 that under 35～70 ℃ temperature the beaker that casting solution is housed carried out the water-bath heating 5～8 hours and with 400～800 rev/mins speed casting solution is stirred simultaneously.
9, the preparation method of a kind of hydrophily according to claim 6 and compaction resistant polyvinylidene fluoride ultrafilter membrane is characterized in that will sticking together in the step 3 that the system of liquid film film support is arranged is that 10～30 ℃, wet-bulb temperature are that 10～30 ℃, relative humidity are to leave standstill evaporation 20～230 seconds under 80～90% the condition at dry-bulb temperature.
10, the preparation method of a kind of hydrophily according to claim 6 and compaction resistant polyvinylidene fluoride ultrafilter membrane is characterized in that will sticking together in the step 4 in the distilled water that 10～35 ℃ of the system of liquid film film support intrusions are arranged and soaked 6～8 minutes.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105694089A (en) * | 2016-04-27 | 2016-06-22 | 山东科技大学 | Preparation method of super-hydrophilic PET membrane material |
| CN110787487A (en) * | 2019-11-14 | 2020-02-14 | 中国石油大学(华东) | Sea urchin-shaped microsphere modified oil-water separation metal net film and preparation method thereof |
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2007
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105694089A (en) * | 2016-04-27 | 2016-06-22 | 山东科技大学 | Preparation method of super-hydrophilic PET membrane material |
| CN110787487A (en) * | 2019-11-14 | 2020-02-14 | 中国石油大学(华东) | Sea urchin-shaped microsphere modified oil-water separation metal net film and preparation method thereof |
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