CN105797591A - Preparation method of super-hydrophobic polyvinylidene fluoride micro-porous film - Google Patents
Preparation method of super-hydrophobic polyvinylidene fluoride micro-porous film Download PDFInfo
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- CN105797591A CN105797591A CN201610181759.3A CN201610181759A CN105797591A CN 105797591 A CN105797591 A CN 105797591A CN 201610181759 A CN201610181759 A CN 201610181759A CN 105797591 A CN105797591 A CN 105797591A
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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
- B01D69/02—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
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/30—Polyalkenyl halides
- B01D71/32—Polyalkenyl halides containing fluorine atoms
- B01D71/34—Polyvinylidene fluoride
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2323/00—Details relating to membrane preparation
- B01D2323/04—Hydrophobization
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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
- B01D2325/38—Hydrophobic membranes
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- Engineering & Computer Science (AREA)
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- Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
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- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention belongs to the technical field of film separation, and particularly discloses a preparation method of a super-hydrophobic polyvinylidene fluoride micro-porous film.The method includes the following steps of firstly, dispersing graphene and nanosilicon dioxide in polar aprotic solvent to be subjected to ultrasonic treatment for 3-20 hours to obtain a dispersing solution; secondly, dissolving polyvinylidene fluoride and polyvinylpyrrolidone in the dispersing solution at a temperature of 20-80 DEG C to be stirred for 3-48 hours and then subjected to ultrasonic treatment for 1-5 hours to obtain a uniform film casting solution; thirdly, coating with the film casting solution through a film scraper to generate a primary film, soaking the primary film in a quench bath for 0-3 hours, and transferring the primary film into a deionized water bath to be soaked for 2-8 days to be cured into a film, and naturally airing the film to obtain the super-hydrophobic polyvinylidene fluoride micro-porous film.The method is friendly to the environment, mild in reaction conduction and simple; the prepared micro-porous film has the film surface water contact angle of 158+/-1 degrees, has high compression resistance and high hydrophobicity and lipophilicity, and has good application prospects in the field of petrochemical engineering.
Description
[technical field]
The invention belongs to technical field of membrane separation, specifically a kind of super-hydrophobicity polyvinylidene fluoride microporous film
Preparation method.
[background technology]
Membrane separation technique is high, without phase transformation, simple to operate, non-secondary pollution, separation product due to separation efficiency
The easily advantage such as recoverys, energy-conserving and environment-protective, membrane separation technique is in water demineralizing and purification, petrochemical industry, gently
Work, weaving, food, biotechnology, medicine and other fields are applied.Membrane material is as membrane separation technique
Core, its character and structure play conclusive effect to the performance of membrance separation.
Kynoar (PVDF) is a kind of crystalline polymer of the chain with-CH2-CF2-as construction unit,
In crystalline structure, carbochain indention arranges, after hydrogen atom is replaced by the fluorine atom that electronegativity is bigger, with
Adjacent fluorine atom is mutually exclusive, so that fluorine atom is the most in the same plane, and divides along carbochain as spiral
Cloth, therefore surrounded by the fluorine atom that series of properties is stable in carbochain surrounding, the most gapless this space
Destroyed carbochain in barrier makes any atom or group can not enter its structure easily.Just because of this
Structure so that PVDF has the excellent chemical stabilities such as the acid and alkali resistance of excellence, oxidant, heat stability
With features such as easy film forming, it is widely used in the preparation of membrane material, is applied especially to the preparation of microporous membrane.
Term " super-hydrophobic " is interpreted as such surface character, water droplet and described surface on described surface
Form becomes the contact angle more than or equal to 150 °.Pvdf membrane inherently has higher hydrophobic performance, in recent years
Carry out most researcheres and often pvdf membrane is modified as hydrophilic, and have ignored himself hydrophobic performance at oil
The application in the fields such as work, the research to its hydrophobic performance is less.
[summary of the invention]
Present invention aim to solve above-mentioned deficiency, utilize the hydrophobic performance of Kynoar, it is provided that
The preparation method of a kind of super-hydrophobicity polyvinylidene fluoride microporous film, separates the anti-pressure ability of film, separation to improve
Efficiency and service life.
Design the preparation method of a kind of super-hydrophobicity polyvinylidene fluoride microporous film for achieving the above object, including with
Lower step: (1) Graphene and the preparation of nano silicon dispersion liquid: first weigh a certain amount of Graphene and
Nano silicon is scattered in polar non-solute, and supersound process 3-20h obtains dispersion liquid;(2) casting
The preparation of film liquid: first weigh a certain amount of Kynoar and polyvinylpyrrolidone, more successively by polyethylene
The dispersion liquid that ketopyrrolidine and Kynoar addition step (1) prepare stirs, obtains casting solution,
By standby for ultrasonic for casting solution deaeration 1-5h;(3) immersion precipitation phase inversion process film forming: step (2) is prepared
Casting solution by blade applicator blade coating generate primary membrane, primary membrane is immersed in coagulation bath, to be filmed after take
Going out to immerse in deionized water 2-8 days, period changes a water every 5-12h, finally dries, and i.e. obtains super thin
Aqueous polyvinylidene fluoride microporous film.
As preferably, in step (1), described polar non-solute is DMF, N, N-
Dimethyl acetylamide, N-Methyl pyrrolidone or triethyl phosphate.
Further, the weight ratio of described Kynoar, polyvinylpyrrolidone, polar non-solute
For (10-18): (2-5): (70-84).
Further, described Graphene, nano silicon, the weight ratio of Kynoar are (0.01-0.1):
(1-4): (10-18).
Further, in step (2), whipping temp is 30-90 DEG C, and mixing time is 6-48h.
Further, in step (3), described coagulation bath is the ethanol solution of 0.1-60wt%.
Further, in step (3), the primary membrane that described casting solution is formed at coagulation bath Immersion time is
0-30min, is 3-7 days at deionized water Immersion time.
Further, in step (3), the temperature of described coagulation bath is 20-30 DEG C, the temperature of deionized water
For 20-40 DEG C.
The present invention compared with the existing technology, has the advantage that
(1) by controlling Graphene, nano silicon, polyvinylpyrrolidone and polar non-solute
Proportion, prepare super-hydrophobicity polyvinylidene fluoride microporous film, this microporous membrane film surface with the contact angle of water is
158 ± 1 ° of its compressive properties are good, have good hydrophobic oleophilic oil;
(2) hydrophobic performance of Kynoar is utilized, the super-hydrophobicity polyvinylidene fluoride microporous film provided
Preparation method, it is possible to increase separate the anti-pressure ability of film, separation efficiency and service life;
(3) method environmental friendliness of the present invention, reaction condition gentleness, preparation method are simply, at oil
The fields such as chemical industry have a good application prospect.
[accompanying drawing explanation]
Fig. 1 is the surface structure scanning electron microscope (SEM) photograph that embodiment 1 prepares super-hydrophobicity polyvinylidene fluoride microporous film;
Fig. 2 is the surface structure scanning electron microscope (SEM) photograph that embodiment 2 prepares super-hydrophobicity polyvinylidene fluoride microporous film;
Fig. 3 is the surface structure scanning electron microscope (SEM) photograph that embodiment 3 prepares super-hydrophobicity polyvinylidene fluoride microporous film.
[detailed description of the invention]
The invention provides the preparation method of a kind of super-hydrophobicity polyvinylidene fluoride microporous film, comprise the following steps:
(1) Graphene and the preparation of nano silicon dispersion liquid: first weigh a certain amount of Graphene and nanometer
Silicon dioxide is scattered in polar non-solute, and supersound process 3-20h obtains dispersion liquid, wherein, and polarity
Aprotic solvent is N,N-dimethylformamide, DMAC N,N' dimethyl acetamide, N-Methyl pyrrolidone or phosphoric acid
Triethyl;
(2) preparation of casting solution: first weigh a certain amount of Kynoar and polyvinylpyrrolidone, more first
After polyvinylpyrrolidone and Kynoar added in the dispersion liquid that step (1) prepares stir, stir
Mixing temperature and be 30-90 DEG C, mixing time is 6-48h, obtains casting solution, by ultrasonic for casting solution deaeration 1-5h
Standby, wherein, Kynoar, polyvinylpyrrolidone, the weight ratio of polar non-solute are (10-18):
(2-5): (70-84), Graphene, nano silicon, the weight ratio of Kynoar are (0.01-0.1):
(1-4): (10-18);
(3) immersion precipitation phase inversion process film forming: the casting solution that step (2) prepares is scratched by blade applicator
Generating primary membrane, primary membrane is immersed in 0-30min in coagulation bath, the temperature of coagulation bath is 20-30 DEG C, should
Coagulation bath is the ethanol solution of 0.1-60wt%, to be filmed after take out and immerse in deionized water 2-8 days, preferably
3-7 days, the temperature of deionized water was 20-40 DEG C, and period changes a water every 5-12h, finally dries, i.e.
Obtain super-hydrophobicity polyvinylidene fluoride microporous film.
The present invention is made further explained below below in conjunction with specific embodiment:
Embodiment 1
(1) Graphene and the preparation of nano silicon dispersion liquid: first weigh 10mg Graphene and 1g nanometer two
Silicon oxide is scattered in the DMF solvent of 70g, supersound process 8 hours, obtains dispersion liquid
Standby;
(2) preparation of casting solution: weigh 10g Kynoar respectively and 2g polyvinylpyrrolidone is dissolved in dispersion
In liquid, at 60 DEG C, stir 12h, ultrasonic 1h obtain casting solution;
(3) immersion precipitation phase inversion process film forming: scrape on glass by casting solution blade applicator, stops in air
10s, is then placed in 40wt% ethanol coagulation bath submergence 10min, to be filmed after take out and immerse in deionized water 3
My god, period changes a water every 6h, finally dries and obtains super-hydrophobicity polyvinylidene fluoride microporous film, uses liquid
It is 148 ° that dripping method records surface contact angle, takes dry film and the surface of film is carried out electron-microscope scanning, obtain Fig. 1.
Embodiment 2
(1) Graphene and the preparation of nano silicon dispersion liquid: first weigh 55mg Graphene and 2.5g nanometer
Silicon dioxide is scattered in the DMF solvent of 77g, and supersound process 3h obtains dispersion liquid standby
With;
(2) preparation of casting solution: weigh 14g Kynoar respectively and 3.5g polyvinylpyrrolidone is dissolved in
In dispersion liquid, at 30 DEG C, stir 6h, ultrasonic 1h obtain casting solution;
(3) immersion precipitation phase inversion process film forming: scrape on glass by casting solution blade applicator, stops in air
5s, is then placed in 60wt% ethanol coagulation bath submergence 30min, to be filmed after take out and immerse in deionized water 2 days,
Period changes a water every 6h, finally dries and obtains super-hydrophobicity polyvinylidene fluoride microporous film, uses sessile drop method
Recording surface contact angle is 158 °, takes dry film and the surface of film is carried out electron-microscope scanning, obtain Fig. 2.
Embodiment 3
(1) Graphene and the preparation of nano silicon dispersion liquid: first weigh 100mg Graphene and 4g nanometer
Silicon dioxide is scattered in the triethyl phosphate solvent of 84g, and supersound process 12h obtains dispersion liquid standby;
(2) preparation of casting solution: weigh 18g Kynoar powder respectively and 5g polyvinylpyrrolidone is molten
In dispersion liquid, at 60 DEG C, stir 12h, ultrasonic 5h obtain casting solution;
(3) immersion precipitation phase inversion process film forming: scrape on glass by casting solution blade applicator, stops in air
10s, is then placed in 40wt% ethanol coagulation bath submergence 20min, to be filmed after take out and immerse in deionized water 7
My god, period changes a water every 6h, finally dries and obtains super-hydrophobicity polyvinylidene fluoride microporous film, uses liquid
It is 142 ° that dripping method records surface contact angle, takes dry film and the surface of film is carried out electron-microscope scanning, obtain Fig. 3.
Embodiment 4
(1) Graphene and the preparation of nano silicon dispersion liquid: first weigh 50mg Graphene and 2g nanometer two
Silicon oxide is scattered in the N,N-dimethylacetamide solvent of 75g, and supersound process 20h obtains dispersion liquid standby
With;
(2) preparation of casting solution: weigh 15g Kynoar respectively and 4g polyvinylpyrrolidone is dissolved in point
Dissipate in liquid, at 90 DEG C, stir 12h, ultrasonic 2h obtain casting solution;
(3) immersion precipitation phase inversion process film forming: scrape on glass by casting solution blade applicator, stops in air
10s, is then placed in 40wt% ethanol coagulation bath submergence 10min, to be filmed after take out and immerse in deionized water 8
My god, period changes a water every 6h, finally dries and obtains super-hydrophobicity polyvinylidene fluoride microporous film, uses liquid
It is 136 ° that dripping method records surface contact angle.
Embodiment 5
(1) Graphene and the preparation of nano silicon dispersion liquid: first weigh 60mg Graphene and 2g nanometer two
Silicon oxide is scattered in the N-Methyl pyrrolidone solvent of 80g, and supersound process 18h obtains dispersion liquid standby;
(2) preparation of casting solution: weigh 14g Kynoar respectively and 4g polyvinylpyrrolidone is dissolved in point
Dissipate in liquid, at 60 DEG C, stir 48h, ultrasonic 1h obtain casting solution;
(3) immersion precipitation phase inversion process film forming: scrape on glass by casting solution blade applicator, stops in air
10s, is then placed in 60wt% ethanol coagulation bath submergence 10min, to be filmed after take out and immerse in deionized water 3
My god, period changes a water every 6h, finally dries and obtains super-hydrophobicity polyvinylidene fluoride microporous film, uses liquid
It is 138 ° that dripping method records surface contact angle.
The present invention is not limited by above-mentioned embodiment, other any spirit without departing from the present invention
With the change made under principle, modify, substitute, combine, simplify, all should be the substitute mode of equivalence, all
Within being included in protection scope of the present invention.
Claims (8)
1. the preparation method of a super-hydrophobicity polyvinylidene fluoride microporous film, it is characterised in that include following step
Rapid:
(1) Graphene and the preparation of nano silicon dispersion liquid: first weigh a certain amount of Graphene and nanometer
Silicon dioxide is scattered in polar non-solute, and supersound process 3-20h obtains dispersion liquid;
(2) preparation of casting solution: first weigh a certain amount of Kynoar and polyvinylpyrrolidone, more first
After polyvinylpyrrolidone and Kynoar are added in the dispersion liquid that step (1) prepares and stir,
To casting solution, by standby for ultrasonic for casting solution deaeration 1-5h;
(3) immersion precipitation phase inversion process film forming: the casting solution that step (2) prepares is scratched by blade applicator
Generate primary membrane, primary membrane be immersed in coagulation bath, to be filmed after take out and immerse in deionized water 2-8 days,
Period changes a water every 5-12h, finally dries, and i.e. obtains super-hydrophobicity polyvinylidene fluoride microporous film.
2. the preparation method of super-hydrophobicity polyvinylidene fluoride microporous film as claimed in claim 1, its feature exists
In: in step (1), described polar non-solute is DMF, N, N-dimethylacetamide
Amine, N-Methyl pyrrolidone or triethyl phosphate.
3. the preparation method of super-hydrophobicity polyvinylidene fluoride microporous film as claimed in claim 1 or 2, it is special
Levy and be: described Kynoar, polyvinylpyrrolidone, the weight ratio of polar non-solute are (10-18):
(2-5):(70-84)。
4. the preparation method of super-hydrophobicity polyvinylidene fluoride microporous film as claimed in claim 3, its feature exists
In: described Graphene, nano silicon, the weight ratio of Kynoar are (0.01-0.1): (1-4):
(10-18)。
5. the preparation method of super-hydrophobicity polyvinylidene fluoride microporous film as claimed in claim 4, its feature exists
In: in step (2), whipping temp is 30-90 DEG C, and mixing time is 6-48h.
6. the preparation method of super-hydrophobicity polyvinylidene fluoride microporous film as claimed in claim 5, its feature exists
In: in step (3), described coagulation bath is the ethanol solution of 0.1-60wt%.
7. the preparation method of super-hydrophobicity polyvinylidene fluoride microporous film as claimed in claim 6, its feature exists
In: in step (3), the primary membrane that described casting solution is formed is 0-30min at coagulation bath Immersion time,
Deionized water Immersion time is 3-7 days.
8. the preparation method of super-hydrophobicity polyvinylidene fluoride microporous film as claimed in claim 7, its feature exists
In: in step (3), the temperature of described coagulation bath is 20-30 DEG C, and the temperature of deionized water is 20-40 DEG C.
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CN108246125A (en) * | 2018-02-26 | 2018-07-06 | 三达膜科技(厦门)有限公司 | A kind of high resistance tocrocking inner support Pvdf Microporous Hollow Fiber Membrane and preparation method thereof |
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