CN104368247B - High-molecular porous film, its preparation method and the application of hydrophilic oleophobic under water - Google Patents
High-molecular porous film, its preparation method and the application of hydrophilic oleophobic under water Download PDFInfo
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- CN104368247B CN104368247B CN201310351517.0A CN201310351517A CN104368247B CN 104368247 B CN104368247 B CN 104368247B CN 201310351517 A CN201310351517 A CN 201310351517A CN 104368247 B CN104368247 B CN 104368247B
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Abstract
The invention discloses a kind of hydrophilic perforated membrane of oleophobic macromolecular under water, its preparation method and application.This hydrophilic perforated membrane of oleophobic macromolecular under water is macromolecular material matrix membrane, film surface has the porous coarse structure of micro-nano size, inside is distributed nanoscale, micron order and/or submicron order duct, wherein this hydrophilic porous film surface of oleophobic macromolecular under water is to the static contact angle of water less than 10 °, under water the static contact angle of oil is more than 130 °.The hydrophilic perforated membrane of oleophobic macromolecular under water of the present invention can be used for separating the oil water mixture produced with purification process Chemical Manufacture, daily life, oil spill disaster etc. and emulsifying profit, has important using value and is widely applied field.
Description
Technical field
The invention belongs to field of material technology, particularly to a kind of hydrophilic-under water oleophobic high-molecular porous film, it prepares
Method and application.
Background technology
A lot of industries and enterprise such as leather, petrochemical industry, smelting, food processing etc. can produce substantial amounts of emulsifying in process of production
Oil waste water (significant proportion is oil-in-water emulsified waste water), this kind of waste component is complicated, and COD value is high, serious harm water body environment and
Human health, it is therefore necessary to emulsifiable oil waste water is carried out isolation of purified so that it is reach discharge standard.But, use conventional process
Method such as centrifuging, ultrasonic method, air supporting method, coagulation method, oxidizing process etc., separating effect and efficiency are the most relatively low, and may produce
Secondary pollution.Membrane separation technique energy consumption is low, separation efficiency is high, do not have secondary pollution, the most progressively for emulsifiable oil waste water
Isolation of purified.
But, when using membrane separation technique to process emulsifying profit, owing to film surface contamination and concentration polarization easily cause
Separate the blocking of fenestra road so that flux and separation efficiency rapid decrease, it is difficult to meet actual requirement.Each for solving in emulsifying profit
Class component (including oil point, surfactant, auxiliary agent etc.), in the problem separating film absorption pollution and cause separation efficiency to decline, is ground
Study carefully personnel and carry out hydrophilic modifying to separating film, as grafting functional group and hydrophilic substance be blended, surface self-organization, hydrophilic-hydrophobic
Block copolymerization etc., but antipollution effect is unsatisfactory.In recent years, there is special infiltrating separation film to receive significant attention.
But, having special infiltrating separation film at present can only be relatively big (generally higher than 20 microns) to the particle diameter in oil slick waste water system
Oil slick separate, and can not the less oil emulsion of particle separation diameter.Meanwhile, this kind of separation film-strength is the most poor, also becomes to be limited
Make one of its wide variety of factor.
Summary of the invention
For solving the problems referred to above, the invention provides the high-molecular porous film its preparation method of a kind of hydrophilic-oleophobic under water
And application.This high-molecular porous film have fast to water infiltration speed, be difficult to the characteristics such as pollution, to oil water mixture and containing micron
It is respectively provided with higher separation efficiency with the oil hydrosol of nano-scale emulsion droplets and separates flux, and its preparation method is easy,
Cost of manufacture is low, be suitable for large area batch preparation.
For achieving the above object, present invention employs following technical scheme:
A kind of hydrophilic-under water oleophobic macromolecular perforated membrane be macromolecular material matrix membrane, film surface has micro-nano size
Porous coarse structure, inside is distributed nanoscale, micron order and/or submicron order duct, wherein this is hydrophilic-under water oleophobic high
Molecule porous diaphragm surface is less than 10 ° to the static contact angle of water, under water the static contact angle of oil is more than 130 °.
One of preferably, described macromolecular material is selected from Kynoar, politef, polypropylene, gathers
Any one in vinyl chloride, polystyrene and polyether sulfone；Described macromolecular material grafting hydrophilic functional group includes polypropylene
Acid and derivant, poly-N-ethyl acetamide, polymethacrylates, polystyrene-b-polyacrylic acid, polysulfonate.
The most hydrophilic-under water the preparation method of oleophobic macromolecular perforated membrane include:
Macromolecular material is dissolved in organic solvent and prepares macromolecule material solution；
Described macromolecular solution is transferred to substrate surface carry out sprawling or direct fabrics molding；
The inversion of phases induced by salts substances obtains hydrophilic-oleophobic macromolecular perforated membrane under water.
One of preferably, the concentration of described macromolecule material solution is 0.05～40 weight %.
One of preferably, the method for the inversion of phases of described salts substances induction is by surface is had macromolecule
The substrate of film is placed in the coagulating bath of described salts substances and carries out inversion of phases.
Wherein, the concentration of described salts substances is preferably 1～50 weight %.
One of preferably, described macromolecular solution is transferred to substrate surface and carries out sprawling or direct fabrics molding
Method be hollow fiber spinning, rejection film method, coating method, note embrane method or scrape embrane method.
One of preferably, described salts substances is selected from inorganic salt, such as potassium nitrate, copper chloride, sodium chloride, chlorination
Potassium, magnesium sulfate；Organic salt, such as sodium acetate, sodium benzoate, tributyl ammonium nitrate, N-alkyl pyridine hydrochlorate, Tetrafluoroboric acid four
The most own ammonium.
The most hydrophilic-under water oleophobic macromolecular perforated membrane may be used for oil-water separation.
Compared with prior art, the beneficial effects of the present invention is: the parent that the inversion of phases induced by salts substances is prepared
The oleophobic macromolecular perforated membrane of water-under water has nanometer, micron and/or submicron order duct, it is possible to realize the height to emulsifying profit
Effect separates.The present invention solves the pollution poor, the most adsorbed of common polymeric membrane for separation hydrophilic and has special wetting property
Separate the bigger problem of membrane aperture, there is higher separation efficiency and flux, and its preparation technology operation is simple, can apply
In preparing the large area perforated membrane that thickness is controlled, uniform ground has higher force intensity simultaneously.The present invention hydrophilic-dredge under water
Innage molecule porous diaphragm can be used for the profit separated and purification process Chemical Manufacture, daily life, oil spill disaster etc. produce
Mixture and emulsifying profit, have important using value and be widely applied field.
Accompanying drawing explanation
Fig. 1 is the optical photograph of the hydrophilic-oleophobic macromolecular perforated membrane under water in embodiment 1；
Fig. 2 be in embodiment 1 hydrophilic-under water oleophobic macromolecular perforated membrane to water static contact angle for～0 °；
Fig. 3 be in embodiment 1 hydrophilic-under water oleophobic macromolecular perforated membrane under water to oil (dichloroethanes) Static Contact
Angle is 150 °；
Fig. 4 be in embodiment 1 hydrophilic-under water oleophobic macromolecular perforated membrane SEM figure.
Detailed description of the invention
The problem such as poor, easy pollution in view of polymeric membrane hydrophilic, the present inventor, through studying for a long period of time and putting into practice, uses salt
The inversion of phases technique of material induction has prepared the hydrophilic-oleophobic macromolecular perforated membrane under water of the present invention.This high-molecular porous film table
Mask has nanoscale, micron and/or submicron in having the porous coarse structure of micro/nano level size and this high-molecular porous film
Level duct, wherein this is hydrophilic-under water oleophobic macromolecular porous film surface to the static contact angle of water less than 10 °, under water to oil
Static contact angle more than 130 °, this perforated membrane has the highest separation efficiency to oil water mixture, and (oil-water separation efficiency is universal
More than 99%).
As the preferred embodiments of the present invention, the perforated membrane of the present invention is polymer-based plasma membrane.
Wherein, the material of described high-molecular porous film including, but not limited to Kynoar, politef, poly-third
Alkene, polrvinyl chloride, polystyrene or polyether sulfone etc..Described macromolecular material grafting hydrophilic functional group is including, but not limited to poly-
Acrylic acid and derivant, poly-N-ethyl acetamide, polymethacrylates, polystyrene-b-polyacrylic acid, polysulfonate.
Described salts substances includes but not limited to inorganic salt, such as potassium nitrate, copper chloride, sodium chloride, potassium chloride, magnesium sulfate；Organic salt, as
Sodium acetate, sodium benzoate, tributyl ammonium nitrate, N-alkyl pyridine hydrochlorate, the most own ammonium of Tetrafluoroboric acid four.
The present invention hydrophilic-under water the preparation method of oleophobic macromolecular perforated membrane include:
Macromolecular material is dissolved in organic solvent and prepares macromolecular solution；
Described macromolecular solution is transferred to substrate surface carry out sprawling or direct fabrics molding；
The inversion of phases induced by salts substances obtains hydrophilic-oleophobic macromolecular perforated membrane under water.
Further, it is clear that, foregoing teachings based on this specification, those skilled in the art can be easy to think of
By controlling macromolecular material and the kind of salts substances, concentration (or ratio), macromolecular solution consumption and extension area, and then
Prepare the film of varying strength, thickness and area, use the needs meeting reality application.
Such as, as the preferred embodiment that this is bright, in mixed solution, macromolecular material concentration can be 0.05～40 weight %,
Described macromolecular material grafting hydrophilic functional group includes polyacrylic acid and derivant, poly-N-ethyl acetamide, poly-methyl-prop
Olefin(e) acid ester, polystyrene-b-polyacrylic acid, polysulfonate etc..
As the preferred embodiments of the present invention, hydrophilic-under water the preparation method of oleophobic macromolecular perforated membrane include having as follows
Body step:
Target macromolecule is dissolved in organic solvent and prepares macromolecular solution；
Target salts substances is dissolved in coagulating bath；
Carry out sprawling or direct fabrics molding at substrate surface by macromolecular solution；
Then be placed in the coagulating bath dissolved with target salts substances and carry out inversion of phases, be dried, obtain hydrophilic-dredge under water
Innage molecule porous diaphragm.
Carry out sprawling or the method for direct fabrics molding includes hollow fiber spinning, gets rid of at substrate surface by macromolecular solution
Embrane method, coating method, note embrane method and scrape embrane method.
The present invention hydrophilic-under water oleophobic macromolecular perforated membrane be applied to industry oil-water separation and purification, organic liquid/water
The filtration of system with the field such as separate, but be not limited to this.
Below in conjunction with some preferred embodiments and comparative example, technical scheme is further described.
Embodiment 1
Weigh Kynoar (PVDF, grafted polyacrylic acid, percent grafting 7.1 weight %) and be dissolved in N-Methyl pyrrolidone
(NMP), in, prepare 10mL 0.05g/mL solution, and be stirred until homogeneous.Accurately weigh sodium acetate to be dissolved in pure water, prepare 15 weights
Amount % coagulating bath.By gained macromolecular solution after the glass baseplate surface of pre-wash carries out knifing, proceed to coagulating bath and carry out
Inversion of phases.Then being taken out from coagulating bath by film, drying at room temperature, obtain hydrophilic-oleophobic macromolecular perforated membrane under water, its surface is tied
Structure refers to Fig. 4, and it is 0 ° (refering to Fig. 2) for the contact angle of water, and oil (dichloroethanes) contact angle is 150 ° (refering to figure under water
3)。
Embodiment 2
Weigh polyether sulfone (PES is grafted poly-sodium sulfonate, percent grafting 8.0 weight %) to be dissolved in dimethyl acetylamide (DMAc),
Preparation 200mL 0.17g/mL solution, stirs and ultrasonic deaeration.Accurately weigh potassium nitrate soluble in water, prepare 10 weight %
Coagulating bath.Being transferred in the reactor of small hollow fiber spinning machine by gained macromolecular solution, macromolecular solution is through spinning head
It is directly entered coagulating bath after extrusion and carries out inversion of phases.Then film is taken out from water-bath, 60 DEG C of oven dryings, obtain hydrophilic-water
Lower oleophobic macromolecular perforated membrane.
Embodiment 3
Weigh polystyrene (PS is grafted polymethyl methacrylate, percent grafting 2.5 weight %) and be dissolved in dimethylformamide
(DMF), in, prepare 10mL 0.1g/mL solution, and be stirred until homogeneous.Accurately weigh the most own ammonium of Tetrafluoroboric acid four to be dissolved in pure water,
Prepare 5 weight % coagulating baths.By gained macromolecular solution after the glass baseplate surface of pre-wash carries out film, proceed to solidification
Bath carries out inversion of phases.Then film is taken out from coagulating bath is bathed, drying at room temperature, obtain hydrophilic-oleophobic macromolecular porous under water
Film.
Comparative example 1
Weigh Kynoar (PVDF, grafted polyacrylic acid, percent grafting 7.1 weight %) and be dissolved in N-Methyl pyrrolidone
(NMP), in, 10mL 0.05g/mL homogeneous solution is prepared.Then, after glass baseplate surface carries out knifing, coagulating bath is proceeded to (pure
Water) in carry out inversion of phases.Finally being taken out from coagulating bath by film, in drying at room temperature, i.e. secure satisfactory grades sub-separation film.
Comparative example 2
Weigh polyether sulfone (PES is grafted poly-sodium sulfonate, percent grafting 8.0 weight %) to be dissolved in dimethyl acetylamide (DMAc),
Preparation 200mL 0.17g/mL solution, stirs and ultrasonic deaeration.Gained macromolecular solution is transferred to small hollow fiber
In the reactor of spinning-drawing machine, macromolecular solution is directly entered coagulating bath after spinning head is extruded and carries out inversion of phases.Then by film from
Taking out in water-bath, 60 DEG C of oven dryings, i.e. secure satisfactory grades sub-separation film.
Application examples 1
The high-molecular porous film of Example 1-3 and the separation film of comparative example 1-2, lead to their hydrophilicity, emulsion
Amount and separation efficiency are analyzed comparing.
This test condition is:
(1) test emulsion is SDS/ hexadecane/aqueous systems, is mixed by SDS/ water 1:99 by volume, is subsequently adding
The emulsion (place 3 moonsets under room temperature and occur precipitation) that SDS preparation is uniform and stable.Use observation by light microscope, emulsion grain
Footpath is 2-5 micron.
(2) test pressure is respectively 0.1bar (embodiment 1-3), 1bar (comparative example 1-2).
(3) in filtrate, oil concentration uses the test of TOC method.
Table 1 hydrophilicity compares
| Water contact angle | Oil contact angle under water | |
| Comparative example 1 | 62° | 80° |
| Comparative example 2 | 88° | 70° |
| Embodiment 1 | 5° | 140° |
| Embodiment 2 | 3° | 142° |
| Embodiment 3 | 8° | 139° |
Table 2 emulsion separating property test result
| Water flux, Lm-2h-1 | Oil concentration in filtrate, ppm | |
| Comparative example 1 | 230 | 88 |
| Comparative example 2 | 210 | 80 |
| Embodiment 1 | 1030 | 50 |
| Embodiment 2 | 1150 | 75 |
| Embodiment 3 | 1220 | 65 |
Below it is only the concrete exemplary applications of the present invention, protection scope of the present invention is not constituted any limitation.All employings
The technical scheme that equivalents or equivalence are replaced and formed, within the scope of all falling within rights protection of the present invention.
Claims (8)
1. hydrophilic-oleophobic macromolecular perforated membrane under water, it is characterised in that it is macromolecular material matrix membrane, film surface has
Having the porous coarse structure of micro-nano size, inside is distributed nanoscale, micron order and/or submicron order duct, wherein this parent
The static contact angle of oil less than 10 °, is more than by the oleophobic macromolecular porous film surface of water-under water by the static contact angle of water under water
130°；
Described macromolecular material is selected from Kynoar, politef, polypropylene, polrvinyl chloride, polystyrene and polyether sulfone
In any one or a few；
The graft modification group of described macromolecular material includes polyacrylic acid and derivant, poly-N-ethyl acetamide, poly-methyl
Acrylate, polystyrene-b-polyacrylic acid and polysulfonate.
2. a preparation method for hydrophilic-oleophobic macromolecular perforated membrane under water, including:
Macromolecular material is dissolved in organic solvent and prepares macromolecule material solution；Described macromolecular material selected from Kynoar,
Any one or a few in politef, polypropylene, polrvinyl chloride, polystyrene and polyether sulfone；Described macromolecular material
Grafting hydrophilic functional group includes polyacrylic acid and derivant, poly-N-ethyl acetamide, polymethacrylates, polyphenyl second
Alkene-b-polyacrylic acid, polysulfonate；
Described macromolecular solution is transferred to substrate surface carry out sprawling or direct fabrics molding；
The inversion of phases induced by salts substances obtains hydrophilic-oleophobic macromolecular perforated membrane under water.
Method the most according to claim 2, it is characterised in that described salts substances is selected from potassium nitrate, copper chloride, chlorination
Sodium, potassium chloride, magnesium sulfate, sodium acetate, sodium benzoate, tributyl ammonium nitrate, N-alkyl pyridine hydrochlorate and Tetrafluoroboric acid four
Any one in the most own ammonium.
Method the most according to claim 2, it is characterised in that the concentration of described macromolecule material solution is 0.05～40 weights
Amount %.
Method the most according to claim 2, it is characterised in that the method for the inversion of phases of described salts substances induction is to pass through
Surface has the substrate of polymeric membrane be placed in the coagulating bath of described salts substances and carry out inversion of phases.
Method the most according to claim 5, it is characterised in that the concentration of described salts substances is preferably 1～50 weight %.
Method the most according to claim 2, it is characterised in that described macromolecular solution is transferred to substrate surface and spreads
The method of exhibition or direct fabrics molding includes hollow fiber spinning, rejection film method, coating method, note embrane method and scrapes embrane method.
8. according to described in claim 1 hydrophilic-under water oleophobic macromolecular perforated membrane at oil water mixture, oil hydrosol or contain
Oil waste water isolated and purified in application.
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| CN107096402B (en) * | 2016-02-19 | 2020-03-27 | 中国科学院苏州纳米技术与纳米仿生研究所 | Oil adsorption and adhesion resistant material, film and coating in water, and preparation method and application thereof |
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| CN109261127B (en) * | 2018-08-27 | 2021-08-24 | 浙江工业大学 | Non-selective oleophobic hydrophilic material and preparation method and application thereof |
| CN109503876A (en) * | 2018-11-07 | 2019-03-22 | 江苏金羿射日新材料科技有限公司 | A kind of hydrophilically modified method of hydrophobic material |
| CN110665372B (en) * | 2019-10-18 | 2022-01-25 | 苏州大学 | Porous membrane for micromolecule permeation separation, preparation method and application thereof |
| CN112516807A (en) * | 2020-11-26 | 2021-03-19 | 中国船舶工业系统工程研究院 | Separation membrane, preparation method, aviation kerosene dewatering and purifying method and application |
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