CN106563362A - Preparing method and usage of low-oxidization-degree graphene/zinc oxide nanometer composite film - Google Patents
Preparing method and usage of low-oxidization-degree graphene/zinc oxide nanometer composite film Download PDFInfo
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- CN106563362A CN106563362A CN201610933829.6A CN201610933829A CN106563362A CN 106563362 A CN106563362 A CN 106563362A CN 201610933829 A CN201610933829 A CN 201610933829A CN 106563362 A CN106563362 A CN 106563362A
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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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- 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
- B01D67/0039—Inorganic membrane manufacture
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/02—Inorganic material
- B01D71/021—Carbon
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/02—Inorganic material
- B01D71/024—Oxides
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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
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
Abstract
The invention provides a preparing method and a usage of a low-oxidization-degree graphene/zinc oxide nanometer composite film. The preparing method comprises the following steps: step 1, preparing low-oxidization-degree graphene; step 2, preparing zinc oxide nanorods; and step 3, preparing the low-oxidization-degree graphene/zinc oxide nanometer composite film. According to the low-oxidization-degree graphene/zinc oxide nanometer composite film prepared by the method, a composite dispersion of low-oxidization-degree graphene oxide and the zinc oxide nanorods is prepared based on electrostatic interaction between a low-oxidization-degree graphene oxide sheet and the zinc oxide nanorods, and the low-oxidization-degree graphene/zinc oxide nanometer composite film is finally obtained through suction filtration. The interlayer spacing of the low-oxidization-degree graphene/zinc oxide nanometer composite film is effectively increased, so that the low-oxidization-degree graphene/zinc oxide nanometer composite film has excellent mechanical properties, excellent water flux and stable separating performance. A novel technical means is provided for the removal of dye molecules in water.
Description
Technical field
The invention belongs to technical field of environment function material preparation, refers in particular to a kind of suboxides degree Graphene/zinc-oxide nano
The preparation method and its usage of composite membrane.
Background technology
Waste water from dyestuff is one of main noxious industry waste water, is mainly derived from production industry in the middle of dyestuff and dyestuff, by
The material being lost in and the sewage composition for washing away ground in the mother solution of various products and its intermediate crystallizations, production process.With dye
Material is industrial to go from strength to strength, and its production waste water has become main pollution source of water body.Therefore, how to remove Wastewater Dyes molecule
The always focus and study hotspot of people.
The new and high technology that membrane separation technique is got up because of superiority developments such as its efficient, low energy consumption, inputs easy to operate and low
It is widely used in dye industry.Membrance separation is the separation process based on material, is using each component in mixture
Physics in the material and the difference of chemical property are realizing the detached process of material, therefore membrane material is the base of membrane separation technique
Plinth.
Since single-layer graphene being prepared for by micromechanics stripping method from Geim in 2004 et al., this known most thin carbon
Material has attracted scientific circles with its stable Colloidal particles, superpower mechanical property, excellent electric conductivity and load capacity
Extensive concern and research.Due to Graphene project physicochemical properties, in recent years grapheme material in seperation film should
With having obtained sufficient research (science, 2014,343,740-742).As the oxide of Graphene, the oxidation stone of accumulation
Black alkene had been demonstrated with straightway aquaporin, shows wide application prospect in fields such as water process, ion isolations.
But in actual application, graphene oxide membrane tends not to efficiently separate object.On the one hand it is due to aoxidizing stone
There is black alkene sheet surfaces Coulomb repulsion to cause which form the accumulation horizon of high-sequential, form some inevitable defects
And fold, cause the mechanical performance of graphene oxide seperation film to weaken;On the other hand, graphene oxide layer and layer in aqueous
Between interlamellar spacing can change, more water are embedded in fenestra road, and being given a shock under pressure-driven to cause film
Rupture.Therefore, good mechanical property is prepared, water flux is high, the good ultra-filtration and separation film tool of separating property is of great significance.
Research shows the degree of oxidation by regulating and controlling graphene oxide, thus it is possible to vary oxygen-containing sense in graphene oxide layer
The quantity of group, and then can be on effective control graphene oxide sheet due to the defect and fold produced by oxidizing process
(Appl.Mat.Interfaces,2015,725,13745-13757).Using graphene oxide layer and electronegative nanometer rods
Between electrostatic adsorption, can effectively change the structure of layered graphite oxide alkene film, increase the machinery of graphene oxide membrane
Performance and separating property.
In this technology, prepared by the electrostatic interaction between graphene oxide sheet and zinc oxide nano rod based on suboxides degree
The graphene oxide sheet of suboxides degree and the composite dispersion liquid of zinc oxide nano rod, have been finally given by sucking filtration a kind of low
Graphene oxide/zinc-oxide nano composite membrane, has effectively added the interlamellar spacing of suboxides Graphene/zinc-oxide nano composite membrane, tool
There are more excellent mechanical performance and water flux, and with stable separating property, this removes for dye molecule in water and provides newly
Technological means.
The content of the invention
The purpose of the present invention is to prepare a kind of Graphene of suboxides degree/zinc-oxide nano composite membrane, and the seperation film has
There are excellent mechanical performance and high water flux, can effectively remove dye molecule in aqueous solution.
The present invention is achieved through the following technical solutions:
A kind of preparation method of suboxides degree Graphene/zinc-oxide nano composite membrane, comprises the steps:
The preparation of step 1, the graphene oxide (GO) of suboxides degree
In the beaker of 250mL, by potassium permanganate (KMnO4) it is slowly added into concentrated sulphuric acid (H2SO4) and phosphoric acid (H3PO4) mixed
Close in solution, add graphite powder, magnetic agitation 1min;By mixed solution in ice-water bath ultrasound 1h, it is slow again after reaction plus
Enter deionized water;After vacuum filtration, by filtrate centrifugation, deionized water and dioxygen water washing, that is, obtain suboxides respectively
The GO of degree;
The preparation of step 2, zinc oxide nano rod (ZnO)
A 250mL there-necked flask and Dropping funnel are taken, zinc acetate is added in ethanol, obtain zinc acetate ethanol molten
Liquid;Separately take during sodium hydroxide (NaOH) is added to ethanol and obtain sodium hydroxide ethanol solution, under magnetic stirring, by sodium hydroxide
Ethanol solution is slowly added in zinc acetate ethanol solution by Dropping funnel;After completion of dropping, mixed liquor is transferred to into poly- four
Constant temperature thermal response is carried out in fluorothene reactor;After reaction inverse ratio, centrifugation solid product distinguishes deionized water and ethanol
Washing, the zinc oxide nano rod vacuum drying for obtaining;
The preparation of step 3, suboxides degree Graphene/zinc-oxide nano composite membrane
In beaker, deionized water is added, add the suboxides degree graphene oxide and step 2 of step 1 preparation to prepare
Zinc oxide nano rod, magnetic agitation 30min, ultrasonic 30min;It is 0.45 μm of cellulose mixture film as basement membrane with aperture, vacuum
Sucking filtration, the suboxides Graphene for obtaining/zinc-oxide nano composite membrane vacuum drying.
In step 1, potassium permanganate, concentrated sulphuric acid, phosphoric acid, the mass ratio of graphite powder is 0.2~0.8:6.5~26:13~52:
0.05~0.2g.
In step 2, during configuration zinc acetate ethanol solution, the zinc acetate for being used and the mass volume ratio of ethanol are 255.5
~1022mg:35mL;During configuration sodium hydroxide ethanol solution, the sodium hydroxide for being used and the mass volume ratio of ethanol are 233
~932mg:35mL;The zinc acetate ethanol solution is 1 with sodium hydroxide volumes of aqueous ethanol ratio:1;The constant temperature thermal response
Temperature is 160 DEG C, and the response time is 24h.
In step 3, when configuration suboxides degree graphene oxide is with zinc oxide nano rod mixed solution, the hypoxia for being used
The mass concentration ratio of change degree graphene oxide and zinc oxide nano rod is 0.1~0.4g/L:0.8~3.2g/L.
Prepared suboxides degree Graphene/zinc-oxide nano composite membrane is used to remove dye molecule in eliminating water.
Beneficial effect:
Graphene/zinc-oxide nano the composite membrane of a kind of suboxides degree prepared by the present invention, based on suboxides degree
Electrostatic interaction between graphene oxide sheet and zinc oxide nano rod, is prepared for the graphene oxide and zinc oxide nano of suboxides degree
The composite dispersion liquid of rice rod, has finally given a kind of Graphene of suboxides degree/zinc-oxide nano composite membrane by sucking filtration, has had
The interlamellar spacing that increased suboxides Graphene/zinc-oxide nano composite membrane of effect, with excellent mechanical performance and water flux, and
With stable separating property, this removes for dye molecule in water and provides new technological means.
Description of the drawings
Fig. 1 is the transmission electron microscope picture of the zinc oxide nano rod under different amplification of the preparation in embodiment 1;
X-ray diffractograms of the Fig. 2 for the material in embodiment 1, wherein, (a) X for suboxides degree graphene oxide is penetrated
Ray diffraction diagram, is (b) X-ray diffractogram of suboxides degree graphene oxide/zinc oxide nano rod complex, is (c) hypoxia
The X-ray diffractogram of change degree graphene oxide/zinc oxide nano rod composite membrane;
X-rays of the Fig. 3 for the suboxides degree graphene oxide/zinc oxide nano rod composite membrane of the preparation in embodiment 1
Energy spectrum diagram.
Specific embodiment
With reference to example is embodied as, the present invention will be further described.
Embodiment 1:
(1) the preparation of the graphene oxide (GO) of suboxides degree
In the beaker of 250mL, by 0.4g potassium permanganate (KMnO4) it is slowly added into 13.0g concentrated sulphuric acid (H2SO4) with
26.0g phosphoric acid (H3PO4) in mixed solution, add 0.1g graphite powders, magnetic agitation 1min;By mixed solution in ice-water bath
Ultrasonic 1h, is slow added into 120g deionized waters after reaction;After vacuum filtration, by filtrate centrifugation, difference deionized water
With dioxygen water washing, that is, obtain the GO of suboxides degree.
(2) the preparation of zinc oxide nano rod (ZnO)
A 250mL there-necked flask and Dropping funnel are taken, 511mg zinc acetates are added in 35mL ethanol solution;Separately take
466mg sodium hydroxide (NaOH) is added in 35mL ethanol solution, under magnetic stirring, is passed through Dropping funnel and is slowly added to
To in the ethanol solution of zinc acetate;After completion of dropping, mixed liquor is transferred in 140mL ptfe autoclaves, 160 DEG C of bars
24h is reacted under part;After being cooled to room temperature, centrifugation, respectively deionized water and washing with alcohol twice, the zinc oxide nano for obtaining
Rice rod is vacuum dried 15h at 50 DEG C.
(3) a kind of preparation of the Graphene of suboxides degree/zinc-oxide nano composite membrane
In 50mL beakers, 20mL deionized waters are added, add the suboxides degree graphene oxide and step of step 1 preparation
Rapid 2 zinc oxide nano rods for preparing, magnetic agitation 30min, ultrasonic 30min;It is 0.45 μm of cellulose mixture film as base with aperture
Film, vacuum filtration, the graphene oxide for obtaining/zinc-oxide nano composite membrane are vacuum dried 12h at 60 DEG C.
The random dispersion of a large amount of uniform zinc oxide nano rods be should be apparent that from Fig. 1 (a), figure (b) can be seen
Go out a diameter of 15nm of single zinc oxide nano rod, length reaches 200nm, this explanation is successfully prepared the uniform zinc oxide nano of pattern
Rice rod.
X-ray diffractograms of the Fig. 2 (a) for suboxides degree graphene oxide, in 2 θ=11.01oPlace's appearance one is very strong
Absworption peak, this belongs to the characteristic diffraction peak in (001) face of GO, shows eucolloid graphite powder successful transformation into suboxides journey
Degree graphene oxide;Compared to Fig. 2 (a), from Fig. 2 (b) it can be seen that suboxides degree graphene oxide-zinc-oxide nano is multiple
Compound, 2 θ=31.9 °, 34.3 °, 36.2 °, 47.6 °, 56.6 °, 62.8 °, 67.8 ° and 69.2 ° there is stronger absworption peak, this
Zinc Oxide (100), (002), (101), (102), (110), (103), (112), and the characteristic diffraction peak of (201) are belonged to, and
And the characteristic peak of graphene oxide is remained, this shows the compound complex of suboxides degree graphene oxide/zinc-oxide nano
Successfully prepare;Compared to Fig. 2 (b), Fig. 2 (c) can see that suboxides degree graphene oxide/zinc-oxide nano composite membrane retains
The characteristic peak of graphene oxide and Zinc Oxide, this shows successfully by suboxides degree graphene oxide/zinc oxide composites system
For suboxides degree graphene oxide-Zinc Oxide composite membrane.
The X-ray energy spectrogram of suboxides degree graphene oxide/zinc oxide nano rod composite membrane as can see from Figure 3
In, the signal peak of C, O and Zn is occurred in that respectively, this further illustrates this Success in Experiment and is prepared for suboxides degree graphite oxide
Alkene/zinc oxide nano rod composite membrane.
Embodiment 2:
(1) the preparation of the graphene oxide (GO) of suboxides degree
In the beaker of 250mL, by 0.2g potassium permanganate (KMnO4) it is slowly added into 6.5g concentrated sulphuric acid (H2SO4) and 13g
Phosphoric acid (H3PO4) in mixed solution, add 0.05g graphite powders, magnetic agitation 1min;Mixed solution is ultrasonic in ice-water bath
1h, is slow added into 120g deionized waters after reaction;After vacuum filtration, by filtrate centrifugation, deionized water and double respectively
Oxygen water washing, that is, obtain the GO of suboxides degree.
(2) the preparation of zinc oxide nano rod (ZnO)
A 250mL there-necked flask and Dropping funnel are taken, 255mg zinc acetates are added in 35mL ethanol solution;Separately take
233mg sodium hydroxide (NaOH) is added in 35mL ethanol solution, under magnetic stirring, is passed through Dropping funnel and is slowly added to
To in the ethanol solution of zinc acetate;After completion of dropping, mixed liquor is transferred in 140mL ptfe autoclaves, 160 DEG C of bars
24h is reacted under part;After being cooled to room temperature, centrifugation, respectively deionized water and washing with alcohol twice, the zinc oxide nano for obtaining
Rice rod is vacuum dried 15h at 50 DEG C.
(3) a kind of preparation of the Graphene of suboxides degree/zinc-oxide nano composite membrane
In 50mL beakers, 20mL deionized waters are added, add 0.002g suboxides degree graphene oxides and 0.016g
Zinc oxide nano rod, magnetic agitation 30min, ultrasonic 30min;It is 0.45 μm of cellulose mixture film as basement membrane with aperture, vacuum is taken out
Filter, the suboxides Graphene-zinc-oxide nano composite membrane for obtaining are vacuum dried 12h at 60 DEG C.
Embodiment 3:
(1) the preparation of the graphene oxide (GO) of suboxides degree
In the beaker of 250mL, by 0.8g potassium permanganate (KMnO4) it is slowly added into 26g concentrated sulphuric acid (H2SO4) and 52g phosphorus
Acid (H3PO4) in mixed solution, add 0.2g graphite powders, magnetic agitation 1min;By mixed solution in ice-water bath ultrasound 1h,
120g deionized waters are slow added into after reaction;After vacuum filtration, by filtrate centrifugation, difference deionized water and hydrogen peroxide
Washing, that is, obtain the GO of suboxides degree.
(2) the preparation of zinc oxide nano rod (ZnO)
A 250mL there-necked flask and Dropping funnel are taken, 1022mg zinc acetates are added in 35mL ethanol solution;Separately take
932mg sodium hydroxide (NaOH) is added in 35mL ethanol solution, under magnetic stirring, is passed through Dropping funnel and is slowly added to
To in the ethanol solution of zinc acetate;After completion of dropping, mixed liquor is transferred in 140mL ptfe autoclaves, 160 DEG C of bars
24h is reacted under part;After being cooled to room temperature, centrifugation, respectively deionized water and washing with alcohol twice, the zinc oxide nano for obtaining
Rice rod is vacuum dried 15h at 50 DEG C.
(3) a kind of preparation of the Graphene of suboxides degree/zinc-oxide nano composite membrane
In 50mL beakers, 20mL deionized waters are added, add 0.008g suboxides degree graphene oxides and 0.064g
Zinc oxide nano rod, magnetic agitation 30min, ultrasonic 30min;It is 0.45 μm of cellulose mixture film as basement membrane with aperture, will obtains
Solution vacuum filtration, the graphene oxide for obtaining/zinc-oxide nano composite membrane is vacuum dried 12h at 60 DEG C.
Claims (5)
1. a kind of preparation method of suboxides degree Graphene/zinc-oxide nano composite membrane, it is characterised in that including following step
Suddenly:
The preparation of step 1, suboxides degree graphene oxide
In beaker, during potassium permanganate is slowly added into concentrated sulphuric acid and phosphoric acid mixed solution, graphite powder, magnetic agitation are added
Mix;By adding, the mixed solution of graphite powder is ultrasonic in ice-water bath, and deionized water is slow added into after reaction;Vacuum filtration
Afterwards, by filtrate centrifugation, deionized water and dioxygen water washing, that is, obtain the graphene oxide of suboxides degree respectively;
The preparation of step 2, zinc oxide nano rod
A there-necked flask and Dropping funnel are taken, zinc acetate is added in ethanol, obtain zinc acetate ethanol solution;Hydrogen-oxygen is taken separately
Change during sodium is added to ethanol and obtain sodium hydroxide ethanol solution, under magnetic stirring, sodium hydroxide ethanol solution is passed through into dropping liquid
Funnel is slowly added in zinc acetate ethanol solution;After completion of dropping, mixed liquor is transferred in ptfe autoclave
Row constant temperature thermal response;After reaction inverse ratio, centrifugation solid product distinguishes deionized water and washing with alcohol, the oxidation for obtaining
Zinc nanometer rods are vacuum dried;
The preparation of step 3, suboxides degree Graphene/zinc-oxide nano composite membrane
In beaker, deionized water is added, the oxygen for adding the suboxides degree graphene oxide and step 2 of step 1 preparation to prepare
Change zinc nanometer rods, further ultrasound is mixed after magnetic agitation;It is 0.45 μm of cellulose mixture film as basement membrane with aperture, vacuum is taken out
Filter, the suboxides Graphene for obtaining/zinc-oxide nano composite membrane vacuum drying.
2. the preparation method of a kind of suboxides degree Graphene/zinc-oxide nano composite membrane according to claim 1, which is special
Levy and be, in step 1, potassium permanganate, concentrated sulphuric acid, phosphoric acid, the mass ratio of graphite powder is 0.2~0.8:6.5~26:13~52:
0.05~0.2g;The magnetic agitation time is 1min, and ultrasonic time is 1h.
3. the preparation method of a kind of suboxides degree Graphene/zinc-oxide nano composite membrane according to claim 1, which is special
To levy and be, in step 2, during configuration zinc acetate ethanol solution, the zinc acetate for being used and the mass volume ratio of ethanol be 255.5~
1022mg:35mL;During configuration sodium hydroxide ethanol solution, the sodium hydroxide for being used and the mass volume ratio of ethanol be 233~
932mg:35mL;The zinc acetate ethanol solution is 1 with sodium hydroxide volumes of aqueous ethanol ratio:1;The temperature of the constant temperature thermal response
Spend for 160 DEG C, the response time is 24h;The magnetic agitation time is 30min, and ultrasonic time is 30min.
4. the preparation method of a kind of suboxides degree Graphene/zinc-oxide nano composite membrane according to claim 1, which is special
Levy and be, in step 3, when configuration suboxides degree graphene oxide is with zinc oxide nano rod mixed solution, the hypoxia for being used
The mass concentration ratio of change degree graphene oxide and zinc oxide nano rod is 0.1~0.4g/L:0.8~3.2g/L.
5. suboxides degree Graphene/zinc-oxide nano composite membrane that prepared by the method described in Claims 1 to 4 any one
Purposes, it is characterised in that prepared suboxides degree Graphene/zinc-oxide nano composite membrane is used to remove dyestuff point in eliminating water
Son.
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CN107138048A (en) * | 2017-05-23 | 2017-09-08 | 安徽大学 | A kind of preparation method of the oily seperation film of High-performance graphite oxide alkene/halloysite nanotubes Compound Water |
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 |
CN108159889A (en) * | 2017-12-18 | 2018-06-15 | 江苏大学 | A kind of super hydrophilic-superoleophobic redox graphene filter membrane and purposes |
CN108722206A (en) * | 2018-07-04 | 2018-11-02 | 同济大学 | A kind of antipollution self-cleaning type GO/ZnO-PVDF films and preparation method thereof |
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US11618682B2 (en) | 2019-09-06 | 2023-04-04 | Changzhou Fuxi Technology Co., Ltd | Mixed slurry of strong and weak graphene oxides and preparation method of mixed slurry, and composite film of strong and weak graphene oxides and preparation method of composite film |
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CN110721599B (en) * | 2019-09-24 | 2022-01-11 | 江苏大学 | Preparation method and application of SGO-ZnO-PSF composite ultrafiltration membrane |
WO2021068292A1 (en) * | 2019-10-12 | 2021-04-15 | 浙江大学 | Graphene oxide membrane having tent-shaped structures, preparation method therefor and use thereof |
CN112717719A (en) * | 2020-12-25 | 2021-04-30 | 自然资源部天津海水淡化与综合利用研究所 | Method for preparing graphene oxide composite nanofiltration membrane by spray coating method |
CN114931864A (en) * | 2021-05-08 | 2022-08-23 | 淮阴师范学院 | Two-dimensional material composite separation membrane, preparation method and application |
CN114931864B (en) * | 2021-05-08 | 2023-11-24 | 淮阴师范学院 | Two-dimensional material composite separation membrane, preparation method and application |
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