CN107376657A - Hydrophilic underwater superoleophobic graphite oxide alkenyl filter membrane, preparation method and application - Google Patents
Hydrophilic underwater superoleophobic graphite oxide alkenyl filter membrane, preparation method and application Download PDFInfo
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- CN107376657A CN107376657A CN201710667057.0A CN201710667057A CN107376657A CN 107376657 A CN107376657 A CN 107376657A CN 201710667057 A CN201710667057 A CN 201710667057A CN 107376657 A CN107376657 A CN 107376657A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/02—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor characterised by their properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0079—Manufacture of membranes comprising organic and inorganic components
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/12—Composite membranes; Ultra-thin membranes
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/40—Devices for separating or removing fatty or oily substances or similar floating material
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/24—Mechanical properties, e.g. strength
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/36—Hydrophilic membranes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/48—Antimicrobial properties
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- Environmental & Geological Engineering (AREA)
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- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention provides a kind of hydrophilic underwater superoleophobic graphite oxide alkenyl filter membrane, preparation method and application, epoxy radicals on stannic oxide/graphene nano piece, hydroxyl, the anchored site that carbonyl and carboxyl are embedded in as Kocide SD nano wire, the Kocide SD nano wire that outer surface has hydroxyl is attached on stannic oxide/graphene nano piece by hydrogen bond, Kocide SD nano wire covers, it is interspersed in sheet graphene oxide layer surface and gap, to adjust the surface physical properties of sheet graphene oxide and passage layered structure, form the composite with coarse surface texture and Nanoscale channels structure, positively charged Kocide SD nano wire and negatively charged graphene oxide sheet are tightly deposited on porous membrane by electrostatic interaction, form the hydrophilic underwater superoleophobic graphite oxide alkenyl filter membrane.For water-oil separating, there is the characteristics of excellent hydrophilic and mechanical performance, stability is good, improves preventing membrane pollution performance.
Description
Technical field
The present invention relates to a kind of hydrophilic-underwater superoleophobic graphite oxide alkenyl filter membrane, preparation method and application, belong to point
From membrane preparation technology field.
Background technology
With the mankind to oil development amount be continuously increased and the rapid development of Petroleum Industry, oil and petroleum product make
Dosage is increasing.The thing followed is that a large amount of relative pollutants enter water body environment so as to be formed by different approaches
Petroleum waste water, if these petroleum waste waters not only result in the pollution at soil, water source without processing directly discharge, or even thing can be triggered
Therefore threaten the health of human body.Therefore, carry out going deep into processing by appropriate means for petroleum waste water, urgent need, to reach section
Can, it lower consumption, the purpose that environmental protection and water resource recycle.Membrane separation technique is a new and high technology, by outside energy or
The promotion of chemical potential difference, film is passed through as separating medium using selectivity, two components or multicomponent gas or liquid are separated, divided
Level and enrichment.It has efficient, energy-conservation, and technical process is simple, small investment, pollutes the advantages that small.
Current membrane separation technique is perfect not enough, such as polysulfones polymer film generally existing membrane pollution problem, or mixed
Filter membrane made from closing hydroaropic substance and surface modification, causes treatment effeciency to decline because coating material comes off, and stricter
Experiment condition under the functionalized nano composite filter membrane completed, do not possess Industry Control feature simple to operation.
The content of the invention
For Shortcomings in the prior art, the invention provides a kind of hydrophilic-underwater superoleophobic graphite oxide alkenyl
Filter membrane, preparation method and water-oil separating application, the preparation method are simple and easy.
The present invention is to realize above-mentioned technical purpose by following technological means.
A kind of hydrophilic-underwater superoleophobic graphite oxide alkenyl filter membrane, it is characterised in that：On stannic oxide/graphene nano piece
The anchored site that epoxy radicals, hydroxyl, carbonyl and carboxyl are embedded in as Kocide SD nano wire, outer surface have the hydroxide of hydroxyl
Copper nano-wire is attached on stannic oxide/graphene nano piece by hydrogen bond, the covering of Kocide SD nano wire, is interspersed in sheet oxidation stone
Black alkene sheet surfaces and gap, to adjust the surface physical properties of sheet graphene oxide and passage layered structure, formation has
Coarse surface texture and the composite of Nanoscale channels structure, positively charged Kocide SD nano wire and negatively charged
Graphene oxide sheet is tightly deposited on porous membrane by electrostatic interaction, is formed described hydrophilic-underwater superoleophobic
Graphite oxide alkenyl filter membrane.
Further, the porous membrane is one in acetate fiber adipose membrane, cellulose mixture film, polyvinylidene fluoride film
Kind.
Further, the filter sizes of the porous membrane are 0.22 μm~2 μm.
Further, first, graphene oxide, Kocide SD nano wire are added in distilled water, ultrasonic disperse；Then lead to
The method for crossing vacuum filtration, mixed solution is filtered and deposits to porous membrane surface, it is hydrophilic described in drying-underwater superoleophobic
Graphite oxide alkenyl filter membrane.
Further, the mass ratio of Kocide SD nano wire and graphene oxide is 1：2~6.
Further, the ultrasonic disperse time is 20-60min.
Further, the preparation method of the graphene oxide is to prepare graphite oxide with improvement Hummers methods first, and
Graphite oxide is peeled off using ultrasound, obtains graphene oxide.
Further, the preparation method of the Kocide SD nano wire：0.998g cupric sulfate pentahydrates are added to 20mL distillations
In water, 5-20min is stirred；30mL0.15mol/L ammoniacal liquor is added, places 5-20min；Sodium hydroxide solution is added, reacts 5-
20min；Washing, filtering, drying, collection sample.
Hydrophilic-underwater superoleophobic graphite oxide alkenyl filter membrane is used for water-oil separating.
Graphene oxide (GO) is a kind of most common derivative of graphene, has typical quasi- two-dimensional space structure, its
Surface distributed the carboxyl of the oxygen-containing functional group of substantial amounts of polarity, including the hydroxyl being distributed in face, epoxy radicals and edge, has good
Good hydrophily and mechanical performance.Due to the presence of these groups so that graphene oxide basement membrane can carry out functionalized design,
The chemical modification on surface can change the charge and hydrophilic and hydrophobic of graphene oxide membrane, and the chemical crosslinking inside lamella can adjust film
Lamella gap size.Again by the masking technique such as spraying, spin coating and vacuum filtration can prepare on a large scale thickness it is controllable, point
From excellent performance and the cheap dilute seperation film of graphite oxide of cost.It is special according to the difference of the dilute basement membrane of the graphite oxide of functionalized design
Point, it can be applied to different separation systems.
Cu(OH)2Nano wire has more suitable draw ratio, and is deposited into tridimensional network, has excellent crystallization
Performance, it can be used by one of composition as composite.Due to nanometer Cu (OH)2Skin effect and small size effect
Higher surface-active and contact should be made it have, therefore nano copper hydroxide also has certain bactericidal effect.
The present invention prepares graphene oxide group compound film using cheap graphite material, takes full advantage of two-dimensional structure oxidation
Graphene contains the oxygen-containing functional group of substantial amounts of polarity, has the characteristics of excellent hydrophilic and mechanical performance.With containing hydroxyl
Kocide SD nano wire is enhanced the stability of membrane material, is carried out functionalization to graphene oxide layer and set by Hydrogenbond
Meter, nano wire, which is covered in sheet surfaces, increases roughness, lifts hydrophilic and oleophobic property, and the nano wire regulation interted between lamella is logical
Road structure, expand interlamellar spacing, beneficial to hydrophilic barrier is formed, by oil, water, film three phase separation, lift preventing membrane pollution performance.Using taking out
The method of filter, positively charged Kocide SD nano wire and negatively charged graphene oxide sheet by electrostatic interaction tightly
Ground is deposited on porous membrane, and thickness is easily controlled, difficult for drop-off, and technique is simple.Graphene oxide basement membrane prepared by the present invention
With higher water throughout curve, flux and stability, and the advantages of preventing membrane pollution, oily waste water can be efficiently separated, for oil
Water separation provides a kind of efficient, environmentally friendly and economic technological means, has important practical significance.
Brief description of the drawings
Fig. 1 is the X-ray diffractogram of graphite oxide alkenyl filter membrane of the present invention.
Fig. 2 is graphene oxide and the compound front and rear electron-microscope scanning image of Kocide SD nano wire.
Fig. 3 is common porous filter membrane and oily contact angle test result figure under the graphite oxide alkenyl millipore water.
Fig. 4 is graphene oxide and the compound quality of Kocide SD nano wire is respectively oil under 2,4,6 millipore waters prepared
Contact angle test result figure.
Fig. 5 is the oil-water separation figure of graphite oxide alkenyl filter membrane of the present invention.
Embodiment
Below in conjunction with the accompanying drawings and specific embodiment the present invention is further illustrated, but protection scope of the present invention is simultaneously
Not limited to this.
Embodiment 1
(1) graphene oxide is prepared to improve Hummers methods
Under ice bath state, 3g graphite powders, 40mL concentrated phosphoric acids and 360mL concentrated sulfuric acid magnetic force are added in 500mL three-necked flasks
Stir.Then 18g potassium permanganate is slowly added portionwise, after being sufficiently stirred reaction, three-necked flask is transferred to oil bath from ice bath
And temperature is risen to 50 DEG C and reacts 12 hours while stirs.
Liquid to be mixed is cooled to room temperature and is put into ice-water bath, gradually instills 30% hydrogen peroxide with 1L distilled water dilutings until solution
Glassy yellow is presented.Vacuum filtration filter cake is rinsed with watery hydrochloric acid, and 8000rpm is centrifuged 5 minutes, pickling 3 times, removes the sulfuric acid in solution
Radical ion.10000rpm is centrifuged 10 minutes, washes 5 times, pH value of solution is adjusted into neutrality；Obtain centrifuging vacuum at 60 DEG C of product to do
It is dry.
Products therefrom is dissolved in into distilled water ultrasound to peel off, vacuum drying chamber is dried.
(2) Kocide SD nano wire is prepared
0.998g cupric sulfate pentahydrates are added in 20mL distilled water, stir 15min；It is 0.15mol/L to add 30mL concentration
Ammoniacal liquor, place 15min；The sodium hydroxide solution that 2.88mL concentration is 2.5mol/L is added, reacts 15min；Wash, filter,
Drying, collect sample.
(3) nano material is compound.
Weigh 20 μ g graphene oxides, 40 μ g Kocide SD nano wires, Kocide SD nano wire and graphene oxide quality
Than for 2, adding in 50mL distilled water, ultrasonic disperse 30min.
(4) composite filter membrane is prepared.
By the method for vacuum filtration, mixed solution is filtered and deposits to acetyl cellulose filter membrane surface.In 40 DEG C of bakings
Night drying is placed in case, obtains hydrophilic-underwater superoleophobic graphite oxide alkenyl filter membrane.
Tested through water droplet contact angle in air, the contact of hydrophilic-underwater superoleophobic graphite oxide alkenyl filter membrane of preparation
Angle reaches 54 ° or so；Underwater droplets contact angle test, hydrophilic-underwater superoleophobic graphite oxide alkenyl filter membrane of preparation connect
Feeler reaches 152 ° or so, has good underwater superoleophobic property；By containing diesel oil, chloroform, soya-bean oil oil emulsion exemplified by, it contains
Oily clearance is up to 99%.
Embodiment 2
(1) graphene oxide is prepared to improve Hummers methods
Under ice bath state, 3g graphite powders, 40mL concentrated phosphoric acids and 360mL concentrated sulfuric acid magnetic force are added in 500mL three-necked flasks
Stir.Then 18g potassium permanganate is slowly added portionwise, after being sufficiently stirred reaction, three-necked flask is transferred to oil bath from ice bath
And temperature is risen to 50 DEG C and reacts 12 hours while stirs.
Liquid to be mixed is cooled to room temperature and is put into ice-water bath, gradually instills 30% hydrogen peroxide with 1L distilled water dilutings until solution
Glassy yellow is presented.Vacuum filtration filter cake is rinsed with watery hydrochloric acid, and 8000rpm is centrifuged 5 minutes, pickling 3 times, removes the sulfuric acid in solution
Radical ion.10000rpm is centrifuged 10 minutes, washes 5 times, pH value of solution is adjusted into neutrality；Obtain centrifuging vacuum at 60 DEG C of product to do
It is dry.
Products therefrom is dissolved in into distilled water ultrasound to peel off, vacuum drying chamber is dried.
(2) Kocide SD nano wire is prepared
0.998g cupric sulfate pentahydrates are added in 20mL distilled water, stir 15min；It is 0.15mol/L to add 30mL concentration
Ammoniacal liquor, place 15min；The sodium hydroxide solution that 2.88mL concentration is 2.5mol/L is added, reacts 15min；Wash, filter,
Drying, collect sample.
(3) nano material is compound.
Weigh 20 μ g graphene oxides, 80 μ g Kocide SD nano wires, Kocide SD nano wire and graphene oxide quality
Than for 4, adding in 50mL distilled water, ultrasonic disperse 30min.
(4) composite filter membrane is prepared.
By the method for vacuum filtration, mixed solution is filtered and deposits to mixed ester membranes surface.In 40 DEG C of bakings
Night drying is placed in case, obtains hydrophilic-underwater superoleophobic graphite oxide alkenyl filter membrane.
Tested through water droplet contact angle in air, the contact of hydrophilic-underwater superoleophobic graphite oxide alkenyl filter membrane of preparation
Angle reaches 54 ° or so；Underwater droplets contact angle test, hydrophilic-underwater superoleophobic graphite oxide alkenyl filter membrane of preparation connect
Feeler reaches 152 ° or so, has good underwater superoleophobic property；By containing diesel oil, chloroform, soya-bean oil oil emulsion exemplified by, it contains
Oily clearance is up to 99%.Carry out X-ray diffraction test to it, the graphene oxide of preparation, Kocide SD nano wire all with mark
The characteristic peak of quasi- card is corresponding, and the collection of illustrative plates of composite membrane show that two kinds of materials are successfully compound, and the characteristic peak of graphene oxide from
9.7 ° are displaced to 8.6 °, show that interlamellar spacing is expanded to 1.03nm from 0.91nm.Scanned Electronic Speculum test, it is observed that oxidation stone
Black alkene and Kocide SD successful deposition is covered in surface of graphene oxide to basement membrane surface, Kocide SD nano wire some, increases
Surface roughness is added, some is interspersed in interlayer, improves piece interlayer channel design.
Tested through water droplet contact angle in air, the contact of hydrophilic-underwater superoleophobic graphite oxide alkenyl filter membrane of preparation
Angle reaches 45 ° or so；Underwater droplets contact angle test, hydrophilic-underwater superoleophobic graphite oxide alkenyl filter membrane of preparation connect
Feeler reaches 155 ° or so, has good underwater superoleophobic property；By containing diesel oil, chloroform, soya-bean oil oil emulsion exemplified by, it contains
Oily clearance is up to 99%.
Embodiment 3
(1) graphene oxide is prepared to improve Hummers methods
Under ice bath state, 3g graphite powders, 40mL concentrated phosphoric acids and 360mL concentrated sulfuric acid magnetic force are added in 500mL three-necked flasks
Stir.Then 18g potassium permanganate is slowly added portionwise, after being sufficiently stirred reaction, three-necked flask is transferred to oil bath from ice bath
And temperature is risen to 50 DEG C and reacts 12 hours while stirs.
Liquid to be mixed is cooled to room temperature and is put into ice-water bath, gradually instills 30% hydrogen peroxide with 1L distilled water dilutings until solution
Glassy yellow is presented.Vacuum filtration filter cake is rinsed with watery hydrochloric acid, and 8000rpm is centrifuged 5 minutes, pickling 3 times, removes the sulfuric acid in solution
Radical ion.10000rpm is centrifuged 10 minutes, washes 5 times, pH value of solution is adjusted into neutrality；Obtain centrifuging vacuum at 60 DEG C of product to do
It is dry.
Products therefrom is dissolved in into distilled water ultrasound to peel off, vacuum drying chamber is dried.
(2) Kocide SD nano wire is prepared
0.998g cupric sulfate pentahydrates are added in 20mL distilled water, stir 15min；It is 0.15mol/L to add 30mL concentration
Ammoniacal liquor, place 15min；The sodium hydroxide solution that 2.88mL concentration is 2.5mol/L is added, reacts 15min；Wash, filter,
Drying, collect sample.
(3) nano material is compound.
Weigh 20 μ g graphene oxides, 120 μ g Kocide SD nano wires, Kocide SD nano wire and graphene oxide quality
Than for 6, adding in 50mL distilled water, ultrasonic disperse 30min.
(4) composite filter membrane is prepared.
By the method for vacuum filtration, mixed solution is filtered and deposits to Kynoar filter membrane surface.In 40 DEG C of baking ovens
Middle placement one night drying, obtain hydrophilic-underwater superoleophobic graphite oxide alkenyl filter membrane.
Tested through water droplet contact angle in air, the contact of hydrophilic-underwater superoleophobic graphite oxide alkenyl filter membrane of preparation
Angle reaches 60 ° or so；Underwater droplets contact angle test, hydrophilic-underwater superoleophobic graphite oxide alkenyl filter membrane of preparation connect
Feeler reaches 150 ° or so, has good underwater superoleophobic property；By containing diesel oil, chloroform, soya-bean oil oil emulsion exemplified by, it contains
Oily clearance is up to 99%.
The embodiment is preferred embodiment of the invention, but the present invention is not limited to above-mentioned embodiment, not
Away from the present invention substantive content in the case of, those skilled in the art can make it is any it is conspicuously improved, replace
Or modification belongs to protection scope of the present invention.
Claims (9)
1. hydrophilic-underwater superoleophobic graphite oxide alkenyl filter membrane, it is characterised in that：Epoxy on stannic oxide/graphene nano piece
The anchored site that base, hydroxyl, carbonyl and carboxyl are embedded in as Kocide SD nano wire, the Kocide SD that outer surface has hydroxyl are received
Rice noodles are attached on stannic oxide/graphene nano piece by hydrogen bond, the covering of Kocide SD nano wire, are interspersed in sheet graphene oxide
Sheet surfaces and gap, to adjust the surface physical properties of sheet graphene oxide and passage layered structure, formed with coarse
Surface texture and Nanoscale channels structure composite, positively charged Kocide SD nano wire and negatively charged oxidation
Graphene film is tightly deposited on porous membrane by electrostatic interaction, forms hydrophilic-underwater superoleophobic oxidation
Graphene-based filter membrane.
2. hydrophilic-underwater superoleophobic graphite oxide alkenyl filter membrane according to claim 1, it is characterised in that described more
Hole filter membrane is one kind in acetate fiber adipose membrane, cellulose mixture film, polyvinylidene fluoride film.
3. hydrophilic-underwater superoleophobic graphite oxide alkenyl filter membrane according to claim 1, it is characterised in that described more
The filter sizes of hole filter membrane are 0.22 μm~2 μm.
4. the preparation method of hydrophilic-underwater superoleophobic graphite oxide alkenyl filter membrane according to claim 1, its feature exist
In, first, by graphene oxide, Kocide SD nano wire add distilled water in, ultrasonic disperse；Then the side of vacuum filtration is passed through
Method, mixed solution is filtered and deposits to porous membrane surface, superoleophobic graphite oxide alkenyl hydrophilic described in drying-underwater
Filter membrane.
5. preparation method according to claim 4, it is characterised in that the quality of Kocide SD nano wire and graphene oxide
Than for 1：2~6.
6. preparation method according to claim 4, it is characterised in that the ultrasonic disperse time is 20-60min.
7. preparation method according to claim 4, it is characterised in that the preparation method of the graphene oxide is to use first
Improvement Hummers methods prepare graphite oxide, and peel off graphite oxide using ultrasound, obtain graphene oxide.
8. preparation method according to claim 4, it is characterised in that the preparation method of the Kocide SD nano wire：
0.998g cupric sulfate pentahydrates are added in 20mL distilled water, stir 5-20min；30mL 0.15mol/L ammoniacal liquor is added, is placed
5-20min；Sodium hydroxide solution is added, reacts 5-20min；Washing, filtering, drying, collection sample.
9. superoleophobic graphite oxide alkenyl filter membrane hydrophilic described in claim 1-underwater is used for water-oil separating.
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Cited By (10)
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| CN108014653A (en) * | 2018-01-22 | 2018-05-11 | 福州大学 | A kind of graphene oxide-semiconductor composite film of illumination enhancing water-oil separating performance |
| CN108043246A (en) * | 2017-12-14 | 2018-05-18 | 北京林业大学 | A kind of preparation method for the super hydrophilic organic film impressed based on micro-nano structure surface |
| CN108159889A (en) * | 2017-12-18 | 2018-06-15 | 江苏大学 | A kind of super hydrophilic-superoleophobic redox graphene filter membrane and purposes |
| CN108704489A (en) * | 2018-06-05 | 2018-10-26 | 江苏大学 | Flexible Janus separation membrane for oil-water separation and preparation method and application thereof |
| CN109046036A (en) * | 2018-10-19 | 2018-12-21 | 陈辉昌 | A kind of preparation method of environment-friendly ceramic film |
| CN110180217A (en) * | 2019-05-16 | 2019-08-30 | 西安石油大学 | A kind of graphene-based three-dimensional fiber paper and preparation method thereof for water-oil separating |
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Cited By (13)
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| CN108043246B (en) * | 2017-12-14 | 2021-06-04 | 北京林业大学 | Preparation method of super-hydrophilic organic membrane based on micro-nano structure surface imprinting |
| CN108043246A (en) * | 2017-12-14 | 2018-05-18 | 北京林业大学 | A kind of preparation method for the super hydrophilic organic film impressed based on micro-nano structure surface |
| CN108159889A (en) * | 2017-12-18 | 2018-06-15 | 江苏大学 | A kind of super hydrophilic-superoleophobic redox graphene filter membrane and purposes |
| CN108014653A (en) * | 2018-01-22 | 2018-05-11 | 福州大学 | A kind of graphene oxide-semiconductor composite film of illumination enhancing water-oil separating performance |
| CN108704489A (en) * | 2018-06-05 | 2018-10-26 | 江苏大学 | Flexible Janus separation membrane for oil-water separation and preparation method and application thereof |
| CN108704489B (en) * | 2018-06-05 | 2020-09-25 | 江苏大学 | Preparation method and application of flexible Janus separation membrane for oil-water separation |
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