CN106823829B - A kind of preparation method of super-hydrophobicity pvdf membrane - Google Patents
A kind of preparation method of super-hydrophobicity pvdf membrane Download PDFInfo
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- CN106823829B CN106823829B CN201710103464.9A CN201710103464A CN106823829B CN 106823829 B CN106823829 B CN 106823829B CN 201710103464 A CN201710103464 A CN 201710103464A CN 106823829 B CN106823829 B CN 106823829B
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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
- B01D67/0002—Organic membrane manufacture
- B01D67/0009—Organic membrane manufacture by phase separation, sol-gel transition, evaporation or solvent quenching
- B01D67/0011—Casting solutions therefor
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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
- B01D67/0002—Organic membrane manufacture
- B01D67/0009—Organic membrane manufacture by phase separation, sol-gel transition, evaporation or solvent quenching
- B01D67/0016—Coagulation
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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
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/06—Flat membranes
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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
Abstract
The invention discloses a kind of preparation methods of super-hydrophobic pvdf membrane.This method, which specifically includes that, prepares PVDF casting solution, prepares mixed type coagulating bath；The hollow-fibre membrane for preparing nascent plate membrane or being spun into through hollow spinning head；Above-mentioned primary membrane is stood in air and is placed in coagulating bath, removal residual organic matter is impregnated through deionized water after being fully cured, obtains super-hydrophobicity PVDF composite membrane；The zero defect step pore structure of spherical accumulation is presented by PVDF super-hydrophobic film prepared by this method, the micro-nano dual microtexture of similar lotus leaf surface is presented in surface layer and the internal PVDF microsphere surface being precipitated, therefore not only film surface but also fenestra embody superhydrophobic characteristic, fundamentally improve the anti-wettability energy of film；Super-hydrophobic pvdf membrane preparation method disclosed by the invention has many advantages, such as the simple strong operability of preparation process, avoids the unabiding drawback of resist wet effect of simple film surface modifying super hydrophobicity, is suitable for the membrane process such as membrane distillation, film absorption.
Description
Technical field
The present invention relates to technical field of membrane, more particularly to a kind of preparation method of super-hydrophobic pvdf membrane.
Background technique
It is white powder under Kynoar (PVDF) normality, is a kind of fluorine-containing hydrophobic polymer material.It is protruded
The characteristics of be heat resistance, solubility and high mechanical strength, and there is good chemical stability, at room temperature not by acid, alkali,
Strong oxidizer and halogen are corroded, and can be dissolved in highly polar organic solvent, and colloidal solution is formed.With other hydrophobicity high scores
Sub- material, if PP, PTFE are compared, PVDF because its can by simple non-solvent induce phase transfer method be prepared into microporous barrier by
To attention, but in the membrane contactors operational process such as membrane distillation, infiltration evaporation and film absorption, hydrone enters film caused by fenestra
Wetting phenomena is very serious, to reduce the working efficiency of system, or even causes the paralysis of work system.Therefore PVDF is improved
The hydrophobicity of film, which becomes, pushes its critical issue in the application of membrane contactor field.
The conventional hydrophobic method of pvdf membrane that improves mainly has blending hydrophobic components, film surface hydrophobically modified etc..Patent
A kind of film formula and preparation method thereof of PVDF/ carbon nanotube super-hydrophobic film, the hydridization are disclosed in CN104826503 A
PVDF/ carbon nanotube super-hydrophobic film is obtained after solidifying in nonpolar steam ambient.But carbon nanometer in the film of this method preparation
Pipe can not be exposed in film surface and duct, and nonpolar steam ambient is difficult to control in this method, is not easy to operate, at
Film property decline；Patent CN101474896 A discloses one kind and constructs micro-nano super-hydrophobic coat, this method in film matrix surface
Pvdf membrane surface obtained water droplet contact angle reaches 160 ° or more, but this method can only realize that film surface has super-hydrophobicity,
The hydrophobicity in fenestra road can not inherently be improved；Patent CN105381723 A discloses a kind of system of super-hydrophobic plate membrane
The polyolefin plate basement membrane is carried out the processing of diaphragm hydroxylating first using polyolefin plate membrane as basement membrane by Preparation Method, then sharp
Silanization reaction is carried out on the surface of polyolefin plate basement membrane with silane monomer, it is micro- to construct organosilicon on polyolefin plate basement membrane
Rice or nanostructured surface control silane monomer in polyolefin plate basement membrane by adjusting the water content of Silanization reaction system
Surface direction of polymerization, obtain super-hydrophobic plate membrane.Though this method can be realized the super-hydrophobicity of film surface, fenestra is dredged
Aqueous not promoted, once hydrone enters fenestra, system performance declines rapidly.Therefore film surface and fenestra be can be realized
Synchronization modifying super hydrophobicity can be most important for fundamentally improving the anti-wettability of film.
Super hydrophobic surface can generally be constructed by two methods: one is the structures on the hydrophobic material surface of low-surface-energy
Build micro-nano coarse structure；Another is carried out at modification on micro-nano coarse structure using low-surface energy substance
Reason.Current method for preparing super-hydrophobic surface reported in the literature include sol-gel method, template, electrochemical process, etching method,
Vapour deposition process, LBL self-assembly method, phase separation method, method of electrostatic spinning, spray coating method, solution infusion method etc..
Existing super hydrophobic surface constructing technology, it is raw materials used it is special, process equipment is expensive, operating process is complicated and is difficult to
Control, therefore, the cost that preparation is reduced by innovative approach will be one of the main target of recent research.
Summary of the invention
In order to solve the problems in the existing technology, the present invention provides a kind of preparation method of super-hydrophobicity pvdf membrane,
Overcome the problems, such as the film wetting that hydrophobic membrane encounters in application process in the prior art.
The technical solution adopted by the present invention is that: a kind of preparation method of super-hydrophobicity pvdf membrane, comprising the following steps:
(1) pore-foaming agent: being dispersed in organic solvent by the preparation of PVDF casting solution first, and PVDF powder is dissolved in
It states in organic solvent, constant temperature water bath stirring is then allowed to stand deaeration and obtains uniformly mixed PVDF casting solution；
(2) mixed type coagulating bath is prepared；The mixed type coagulating bath is homogeneous mixed liquor, or be uniformly mixed oil mutually and
The suspension that the emulsion or nanoparticle and organic reagent that water phase is formed are formed；
(3) step (1) casting solution is stopped on supporter with scraper striking at plate membrane and in air, relative humidity
For 40%-70%, temperature is 25-30 DEG C；
(4) plate membrane that step (3) is just made is placed in step (2) and mixed in coagulating bath and solidified；
(5) it is placed on impregnating in deionized water after plate membrane is fully cured, clean, removal is remaining unit
Point, it is drying to obtain the super-hydrophobicity PVDF composite membrane at room temperature.
Step (1) pore-foaming agent is PEG-400, PEG-600 or PVP；The organic solvent is N, N- dimethyl formyl
Amine, N-Methyl pyrrolidone or DMAC N,N' dimethyl acetamide；Bath temperature is controlled at 60-80 DEG C；Time of repose 4-12h.
The homogeneous mixed liquor of the step (2) is the mixed liquor that solvent and water are prepared by a certain percentage；Alcohol and water are by certain ratio
The homogeneous mixed liquor of example mixing.The solvent is n,N-dimethylacetamide, n,N-Dimethylformamide or N- crassitude
Ketone；Alcohols is methanol, ethyl alcohol, normal propyl alcohol, isopropanol or n-butanol.
Step (2) emulsion is finely divided oil, oil emulsion or dissolved oil.In the finely divided oil, oil droplet size is
It 10-100 μm, is suspended in water with tiny oil droplets dispersion；Oil droplet size in oil emulsion is less than 10 μm, mostly at the table of emulsifying
Face activating agent state remains to be stably dispersed in water even if standing a few hours；The partial size of dissolved oil is also smaller than oil emulsion, has
Small to several nanometers.The oil emulsion oil droplet size is 0.1-2.0 μm.
The nanoparticle of step (2) suspension is mainly hydrophobicity graphene or through hydrophobic modified (silylation, fluorine
Fluidized polymer, plasma, the technologies such as chemical graft) Nano-meter SiO_22、TiO2Or carbon nanotube；Organic reagent is N, N- diformazan
Base formamide, N-Methyl pyrrolidone, DMAC N,N' dimethyl acetamide, methanol, ethyl alcohol, normal propyl alcohol, isopropanol or n-butanol.
Step (3) the supporter plate is glass plate or polytetrafluoroethylene (PTFE), and the residence time is 10-60s in air.
Soaking time is 24-48h in step (5) deionized water.
The beneficial effects of the present invention are: that pvdf membrane surface layer and duct is presented is super-hydrophobic for the use of mixed type coagulating bath
Property, to significantly improve the anti-wettability energy of film.Film at the beginning of PVDF is placed in mixed type coagulating bath by the present invention, realizes inversion of phases mistake
The high molecular uneven precipitation of PVDF in journey, so that having obtained one kind has spherical accumulation zero defect step pore structure pvdf membrane,
The PVDF microsphere surface of precipitation has micro-nano dual microtexture, so that film surface and fenestra show superhydrophobic characteristic.The present invention
By simple and easy preparation method be prepared for having it is micro--receive the super-hydrophobic pvdf membrane of dual microtexture, not only realize super thin
Aqueous film surface, while the structure of membrane body is also changed, film wetting can inherently be effectively relieved.
Detailed description of the invention
Fig. 1 is the contact angle of the SEM figure and surface of super-hydrophobic pvdf membrane section made from embodiment 1；
Fig. 2 is the contact angle of the SEM figure and surface of super-hydrophobic pvdf membrane section made from embodiment 2；
Fig. 3 is the contact angle of the SEM figure and surface of super-hydrophobic pvdf membrane section made from embodiment 3.
Specific embodiment
Below in conjunction with drawings and examples, invention is further described in detail.
Embodiment 1
It takes 8.6ml polyethylene glycol-400 to be added in 153mlN- methyl pyrrolidone, is uniformly mixed it.Later will
36gPVDF is added while stirring in above-mentioned solution, and stirring 12h makes it completely dissolved under conditions of 60 DEG C of constant temperature water baths heat,
Uniform casting solution is obtained after standing 12h deaeration in 40 DEG C of vacuum drying ovens；1g graphene is weighed to be added in 1000ml methanol, point
It is added in 2000ml deionized water after dissipating uniformly, coagulating bath is made.Casting solution scraped using scraper prepare on a glass it is nascent
Plate membrane stops 30s in air, then this nascent plate membrane is placed in coagulating bath obtained above until being solidified into
Pvdf membrane；This film is impregnated for 24 hours in deionized water, thoroughly removes solvent remaining in film, drying obtains institute at room temperature
The super-hydrophobic pvdf membrane stated.Test is carried out to pvdf membrane made from embodiment 1 and finds that the film is accumulated by a large amount of microballoon, portion
Microballoon is divided to link together, film surface contact angle reaches 151 °.
Embodiment 2
It takes 9.2ml polyethylene glycol -600 that 165mlN is added, in dinethylformamide, is uniformly mixed it.Later will
40gPVDF is added while stirring in above-mentioned solution, and stirring 12h makes it completely dissolved under conditions of 60 DEG C of constant temperature water baths heat,
Uniform casting solution is obtained after standing 12h deaeration in 40 DEG C of vacuum drying ovens；Weigh 1g alkylation TiO2Nanoparticle is added
It in 1000ml dehydrated alcohol, is added in 1000ml deionized water after being uniformly dispersed, coagulating bath is made.Casting solution is scraped using scraper
Nascent plate membrane is prepared on a glass, 30s is stopped in air, is then placed in this nascent plate membrane obtained above solidifying
Gu until being solidified into pvdf membrane in bath；This film is impregnated for 24 hours in deionized water, is thoroughly removed solvent remaining in film, room
The lower drying of temperature obtains the super-hydrophobic pvdf membrane.Carrying out test to pvdf membrane made from embodiment 2 finds the film by silk ribbon
The polymer of shape is connected to microballoon composition, and microsphere surface is relatively rough, adheres to one layer of nanoparticle, which reaches
158°。
Embodiment 3
It takes 8.6ml polyethylene glycol-400 to be added in 153mlN- methyl pyrrolidone, is uniformly mixed it.Later will
36gPVDF is added while stirring in above-mentioned solution, and stirring 12h makes it completely dissolved under conditions of 60 DEG C of constant temperature water baths heat,
Uniform casting solution is obtained after standing 12h deaeration in 40 DEG C of vacuum drying ovens；Weigh the fluorinated SiO of 1g2Nanoparticle is added
It in 1000mlN- methyl pyrrolidone, is added in 1000ml deionized water after being uniformly dispersed, coagulating bath is made.It will be cast using scraper
Film liquid scrapes and prepares nascent plate membrane on a glass, and 30s is stopped in air, this nascent plate membrane is then placed in above-mentioned system
Until being solidified into pvdf membrane in the coagulating bath obtained；This film is impregnated for 24 hours in deionized water, thoroughly removes solvent remaining in film
It removes, it is dry at room temperature to obtain the super-hydrophobic pvdf membrane.Pvdf membrane made from embodiment 3 is tested, is obtained as follows
As a result: the film by a large amount of rules and coarse spheric granules object is accumulated, nanoparticle it is stable be attached to microsphere surface, shape
At micro-nano dual microtexture, not only this super-hydrophobic dual microtexture is presented in film surface, and fenestra road has also reached super thin
Water, film surface contact angle reach 164 °.
Although above in conjunction with figure, invention has been described, and the invention is not limited to above-mentioned specific embodiment parties
Formula, the above mentioned embodiment is only schematical, rather than restrictive, and those skilled in the art are in this hair
Under bright enlightenment, without deviating from the spirit of the invention, many variations can also be made, these belong to guarantor of the invention
Within shield.
Claims (4)
1. a kind of preparation method of super-hydrophobicity pvdf membrane, which comprises the following steps:
(1) pore-foaming agent: being dispersed in organic solvent by the preparation of PVDF casting solution first, and PVDF powder, which is dissolved in, above-mentioned to be had
In solvent, constant temperature water bath stirring is then allowed to stand deaeration and obtains uniformly mixed PVDF casting solution；
(2) mixed type coagulating bath is prepared；The mixed type coagulating bath is the suspension that nanoparticle and organic reagent are formed；It is described
The nanoparticle of suspension is for hydrophobicity graphene or through hydrophobic modified Nano-meter SiO_22、TiO2Or carbon nanotube；Organic reagent
Be N,N-dimethylformamide, N-Methyl pyrrolidone, DMAC N,N' dimethyl acetamide, methanol, ethyl alcohol, normal propyl alcohol, isopropanol or
N-butanol；
(3) step (1) casting solution is stopped on supporter with scraper striking at plate membrane and in air, relative humidity is
40%-70%, temperature are 25-30 DEG C；
(4) plate membrane that step (3) is just made is placed in step (2) and mixed in coagulating bath and solidified；
(5) it is placed on impregnating in deionized water after plate membrane is fully cured, cleans, remove remaining organic component, room
The super-hydrophobicity PVDF composite membrane is drying to obtain under temperature.
2. the preparation method of super-hydrophobicity pvdf membrane according to claim 1, which is characterized in that step (1) pore-foaming agent
For PEG-400, PEG-600 or PVP；The organic solvent is N,N-dimethylformamide, N-Methyl pyrrolidone or N, N- bis-
Methylacetamide；Bath temperature is controlled at 60-80 DEG C；Time of repose 4-12h.
3. the preparation method of super-hydrophobicity pvdf membrane according to claim 1, which is characterized in that step (3) supporter
Plate is glass plate or polytetrafluoroethylene (PTFE), and the residence time is 10-60s in air.
4. the preparation method of super-hydrophobicity pvdf membrane according to claim 1, which is characterized in that step (5) deionization
Soaking time is 24-48h in water.
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| CN109569325A (en) * | 2019-01-17 | 2019-04-05 | 南京工业大学 | A kind of preparation method of filled-type gradient pore separation membrane |
| CN110152504A (en) * | 2019-06-17 | 2019-08-23 | 沈阳工业大学 | The polyvinylidene fluoride film and preparation method and application of blending and modifying |
| CN110975640B (en) * | 2019-12-13 | 2022-04-01 | 天津工业大学 | Preparation method of three-dimensional hydrophobic tubular nanofiber membrane |
| CN111363269A (en) * | 2020-03-17 | 2020-07-03 | 宁德师范学院 | PVC/PVDF/diatomite composite super-hydrophobic material |
| CN111644067A (en) * | 2020-06-17 | 2020-09-11 | 东北电力大学 | Preparation method of nano micro-column super-amphiphobic composite membrane |
| US11439957B2 (en) | 2020-11-13 | 2022-09-13 | Saudi Arabian Oil Company | Desalination membranes |
| US11571663B2 (en) * | 2020-11-13 | 2023-02-07 | Saudi Arabian Oil Company | Desalination membranes |
| CN112604514B (en) * | 2020-11-17 | 2023-03-14 | 曲靖师范学院 | Super-hydrophobic polyvinylidene fluoride oil-water separation composite membrane and preparation method and application thereof |
| CN115253704B (en) * | 2021-04-29 | 2023-07-21 | 中国石油化工股份有限公司 | Hydrophobic polymer microfiltration membrane and preparation method and application thereof |
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