CN103551052A - Preparation method of super-hydrophobic composite membrane - Google Patents
Preparation method of super-hydrophobic composite membrane Download PDFInfo
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- CN103551052A CN103551052A CN201310531391.5A CN201310531391A CN103551052A CN 103551052 A CN103551052 A CN 103551052A CN 201310531391 A CN201310531391 A CN 201310531391A CN 103551052 A CN103551052 A CN 103551052A
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Abstract
The invention discloses a preparation method of a super-hydrophobic composite membrane. The preparation method comprises the steps of soaking a glass slide into a polyimide sol, then puling out the glass slide, repeating the operations of soaking and pulling out the glass slide for a plurality of times, and drying to obtain a base layer membrane; heating a mixture of polydimethyl siloxane-g-polysulfone and polysulfone hollow fibers to a molten state to obtain a mixed solution, and putting the mixed solution into a container; electrifying the container to jet out polymer flows, and gathering on a receiving plate to obtain a hydrophobic layer; covering the hydrophobic layer on the base layer membrane to obtain the super-hydrophobic composite membrane. Through the way, the super-hydrophobic composite membrane prepared by the preparation method disclosed by the invention is firm in bonding, has very strong hydrophobic property, good mechanical property and relatively high porosity and membrane strength, and the whole preparation process is good in safety performance, little in environmental pollution and simple and easy in operation, and can effectively reduce the production cost.
Description
Technical field
The present invention relates to membrane technology field, particularly relate to a kind of preparation method of super-hydrophobicity composite membrane.
Background technology
Along with constantly advancing of membrane technology, membrane separation technique is also widely used in the various aspects of producing and living.Membrane separation technique can either be recycled utility, can effectively purify waste water again, and membrane separation technique also has the features such as equipment is simple, easy to operate, energy-conservation simultaneously.According to the hydrophilic and hydrophobic of membrane material, film can be divided into hydrophobic film and hydrophilic film, and the film of wherein being made by hydrophobic material is hydrophobic film, and the contact angle that fluid drips forms on film surface is greater than 90 °.The mechanical performance of traditional hydrophobic film is bad, during use, easily ruptures or cracking, and complex manufacturing process, improves production cost greatly.
Summary of the invention
The technical problem that the present invention mainly solves is to provide a kind of preparation method of super-hydrophobicity composite membrane, and the method is safe and reliable, and the film hydrophobic performance obtaining is good.
For solving the problems of the technologies described above, the technical scheme that the present invention adopts is: a kind of preparation method of super-hydrophobicity composite membrane is provided, comprises that step is:
(1) polyimides is dissolved in toluene and constantly and stirs, slowly drip the sodium carbonate liquor that mass percent is 8-10%, described rate of addition is one of every 3-4 second, drips to finish rear continuation and stir 3-5 hour, drip gradually again ammonia spirit and make pH value become alkalescence, obtain polyimides colloidal sol;
(2) slide is immersed in the polyimides colloidal sol that step (1) obtains, soak and put 10-20 minute, with even speed, slide is lifted out from described polyimides colloidal sol, repeated impregnations lifts for several times, take out after described slide in vacuum drying chamber, the temperature setting of described vacuum drying chamber is set to 80-100 ℃, obtains base film layer;
(3) mixture of dimethyl silicone polymer-g-polysulfones and polysulfone hollow fibre is heated to molten condition and obtains mixed liquor, the mass ratio of wherein said dimethyl silicone polymer-g-polysulfones and described polysulfone hollow fibre is 1:1.5-2, and described mixed liquor is put in container;
(4) one end of wire is inserted in described mixed liquor, again the other end of wire is connected with high voltage source, described dimethyl silicone polymer-g-polysulfones and described polysulfone hollow fibre eject formation polymer flow by the shower nozzle of container, described polymer flow is ejected on receiver sheet and carries out enrichment, obtains hydrophobic layer;
(5) described hydrophobic layer is covered on described base film layer, obtain super-hydrophobicity composite membrane.
In a preferred embodiment of the present invention, described in step (1), the mass percent of sodium carbonate liquor is 9%, and continuing mixing time is 4 hours.
In a preferred embodiment of the present invention, described in step (2), the temperature setting of vacuum drying chamber is set to 95 ℃.
In a preferred embodiment of the present invention, described in step (3), the mass ratio of dimethyl silicone polymer-g-polysulfones and described polysulfone hollow fibre is 1:1.7.
The invention has the beneficial effects as follows: the preparation method of super-hydrophobicity composite membrane of the present invention, the super-hydrophobicity composite membrane obtaining is in conjunction with firm, there is very strong hydrophobicity, good mechanical property, have higher porosity and film-strength, whole safe preparation process performance is good, and environmental pollution is little, operation is simple, can effectively reduce production cost.
The specific embodiment
Below the technical scheme in the embodiment of the present invention is clearly and completely described, obviously, described embodiment is only a part of embodiment of the present invention, rather than whole embodiment.Embodiment based in the present invention, those of ordinary skills, not making all other embodiment that obtain under creative work prerequisite, belong to the scope of protection of the invention.
Embodiment mono-:
A kind of preparation method of super-hydrophobicity composite membrane is provided, comprises that step is:
(1) polyimides is dissolved in toluene and constantly and stirs, slowly drip the sodium carbonate liquor that mass percent is 9%, described rate of addition is one of every 4 second, drips and finishes rear continuation stirring 4 hours, drip gradually again ammonia spirit and make pH value become alkalescence, obtain polyimides colloidal sol;
(2) slide is immersed in the polyimides colloidal sol that step (1) obtains, soak and put 15 minutes, with even speed, slide is lifted out from described polyimides colloidal sol, repeated impregnations lifts for several times, take out after described slide in vacuum drying chamber, the temperature setting of described vacuum drying chamber is set to 95 ℃, obtains base film layer;
(3) mixture of dimethyl silicone polymer-g-polysulfones and polysulfone hollow fibre is heated to molten condition and obtains mixed liquor, the mass ratio of wherein said dimethyl silicone polymer-g-polysulfones and described polysulfone hollow fibre is 1:1.7, and described mixed liquor is put in container;
(4) one end of wire is inserted in described mixed liquor, again the other end of wire is connected with high voltage source, described dimethyl silicone polymer-g-polysulfones and described polysulfone hollow fibre eject formation polymer flow by the shower nozzle of container, described polymer flow is ejected on receiver sheet and carries out enrichment, obtains hydrophobic layer;
(5) described hydrophobic layer is covered on described base film layer, obtain super-hydrophobicity composite membrane.
Embodiment bis-:
A kind of preparation method of super-hydrophobicity composite membrane is provided, comprises that step is:
(1) polyimides is dissolved in toluene and constantly and stirs, slowly drip the sodium carbonate liquor that mass percent is 8%, described rate of addition is one of every 3 second, drips and finishes rear continuation stirring 5 hours, drip gradually again ammonia spirit and make pH value become alkalescence, obtain polyimides colloidal sol;
(2) slide is immersed in the polyimides colloidal sol that step (1) obtains, soak and put 17 minutes, with even speed, slide is lifted out from described polyimides colloidal sol, repeated impregnations lifts for several times, take out after described slide in vacuum drying chamber, the temperature setting of described vacuum drying chamber is set to 88 ℃, obtains base film layer;
(3) mixture of dimethyl silicone polymer-g-polysulfones and polysulfone hollow fibre is heated to molten condition and obtains mixed liquor, the mass ratio of wherein said dimethyl silicone polymer-g-polysulfones and described polysulfone hollow fibre is 1:1.5, and described mixed liquor is put in container;
(4) one end of wire is inserted in described mixed liquor, again the other end of wire is connected with high voltage source, described dimethyl silicone polymer-g-polysulfones and described polysulfone hollow fibre eject formation polymer flow by the shower nozzle of container, described polymer flow is ejected on receiver sheet and carries out enrichment, obtains hydrophobic layer;
(5) described hydrophobic layer is covered on described base film layer, obtain super-hydrophobicity composite membrane.
The foregoing is only embodiments of the invention; not thereby limit the scope of the claims of the present invention; every equivalent structure or conversion of equivalent flow process that utilizes description of the present invention to do; or be directly or indirectly used in other relevant technical field, be all in like manner included in scope of patent protection of the present invention.
Claims (4)
1. a preparation method for super-hydrophobicity composite membrane, is characterized in that, comprises that step is:
(1) polyimides is dissolved in toluene and constantly and stirs, slowly drip the sodium carbonate liquor that mass percent is 8-10%, described rate of addition is one of every 3-4 second, drips to finish rear continuation and stir 3-5 hour, drip gradually again ammonia spirit and make pH value become alkalescence, obtain polyimides colloidal sol;
(2) slide is immersed in the polyimides colloidal sol that step (1) obtains, soak and put 10-20 minute, with even speed, slide is lifted out from described polyimides colloidal sol, repeated impregnations lifts for several times, take out after described slide in vacuum drying chamber, the temperature setting of described vacuum drying chamber is set to 80-100 ℃, obtains base film layer;
(3) mixture of dimethyl silicone polymer-g-polysulfones and polysulfone hollow fibre is heated to molten condition and obtains mixed liquor, the mass ratio of wherein said dimethyl silicone polymer-g-polysulfones and described polysulfone hollow fibre is 1:1.5-2, and described mixed liquor is put in container;
(4) one end of wire is inserted in described mixed liquor, again the other end of wire is connected with high voltage source, described dimethyl silicone polymer-g-polysulfones and described polysulfone hollow fibre eject formation polymer flow by the shower nozzle of container, described polymer flow is ejected on receiver sheet and carries out enrichment, obtains hydrophobic layer;
(5) described hydrophobic layer is covered on described base film layer, obtain super-hydrophobicity composite membrane.
2. the preparation method of super-hydrophobicity composite membrane according to claim 1, is characterized in that, described in step (1), the mass percent of sodium carbonate liquor is 9%, and continuing mixing time is 4 hours.
3. the preparation method of super-hydrophobicity composite membrane according to claim 1, is characterized in that, described in step (2), the temperature setting of vacuum drying chamber is set to 95 ℃.
4. the preparation method of super-hydrophobicity composite membrane according to claim 1, is characterized in that, described in step (3), the mass ratio of dimethyl silicone polymer-g-polysulfones and described polysulfone hollow fibre is 1:1.7.
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| CN201310531391.5A CN103551052B (en) | 2013-11-01 | 2013-11-01 | A kind of preparation method of super-hydrophobic composite membrane |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104307387A (en) * | 2014-10-11 | 2015-01-28 | 南京九思高科技有限公司 | Polyvinylidene fluoride-hexafluoropropylene super-hydrophobic composite film and preparation method thereof |
| CN109295717A (en) * | 2018-07-31 | 2019-02-01 | 广州中国科学院先进技术研究所 | A method of quickly preparing oleophobic hydrophobic membrane |
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| US4859215A (en) * | 1988-05-02 | 1989-08-22 | Air Products And Chemicals, Inc. | Polymeric membrane for gas separation |
| US5286280A (en) * | 1992-12-31 | 1994-02-15 | Hoechst Celanese Corporation | Composite gas separation membrane having a gutter layer comprising a crosslinked polar phenyl-containing - organopolysiloxane, and method for making the same - |
| US20100147762A1 (en) * | 2008-12-17 | 2010-06-17 | General Electric Company | Membrane assemblies and methods of making and using the same |
| US20110042315A1 (en) * | 2009-08-19 | 2011-02-24 | University Of Connecticut | Pervaporation composite membrane for aqueous solution separation and methods for using the same |
| CN102294182A (en) * | 2011-07-18 | 2011-12-28 | 清华大学 | Preparation method of hydrophobic nano mesoporous molecular sieve filling PDMC composite film |
| JP2013166131A (en) * | 2012-02-16 | 2013-08-29 | Fujifilm Corp | Composite separation membrane, and separation membrane module using the same |
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2013
- 2013-11-01 CN CN201310531391.5A patent/CN103551052B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4859215A (en) * | 1988-05-02 | 1989-08-22 | Air Products And Chemicals, Inc. | Polymeric membrane for gas separation |
| US5286280A (en) * | 1992-12-31 | 1994-02-15 | Hoechst Celanese Corporation | Composite gas separation membrane having a gutter layer comprising a crosslinked polar phenyl-containing - organopolysiloxane, and method for making the same - |
| US20100147762A1 (en) * | 2008-12-17 | 2010-06-17 | General Electric Company | Membrane assemblies and methods of making and using the same |
| US20110042315A1 (en) * | 2009-08-19 | 2011-02-24 | University Of Connecticut | Pervaporation composite membrane for aqueous solution separation and methods for using the same |
| CN102294182A (en) * | 2011-07-18 | 2011-12-28 | 清华大学 | Preparation method of hydrophobic nano mesoporous molecular sieve filling PDMC composite film |
| JP2013166131A (en) * | 2012-02-16 | 2013-08-29 | Fujifilm Corp | Composite separation membrane, and separation membrane module using the same |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104307387A (en) * | 2014-10-11 | 2015-01-28 | 南京九思高科技有限公司 | Polyvinylidene fluoride-hexafluoropropylene super-hydrophobic composite film and preparation method thereof |
| CN109295717A (en) * | 2018-07-31 | 2019-02-01 | 广州中国科学院先进技术研究所 | A method of quickly preparing oleophobic hydrophobic membrane |
| CN109295717B (en) * | 2018-07-31 | 2021-04-27 | 广州中国科学院先进技术研究所 | Method for rapidly preparing oleophobic hydrophobic membrane |
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| CN103551052B (en) | 2015-07-29 |
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Effective date of registration: 20160527 Address after: 214000 No. 9, Mount Huangshan Road, Xin Wu District, Jiangsu, Wuxi Patentee after: Wuxi and Shuo Feng new material Co. Ltd. Address before: 214000 Jiangsu Province, Wuxi city Huishan District Road No. 63 East Street Yuqi Patentee before: Wuxi Hai Te new material research institute Co., Ltd |