CN103551052B - A kind of preparation method of super-hydrophobic composite membrane - Google Patents
A kind of preparation method of super-hydrophobic composite membrane Download PDFInfo
- Publication number
- CN103551052B CN103551052B CN201310531391.5A CN201310531391A CN103551052B CN 103551052 B CN103551052 B CN 103551052B CN 201310531391 A CN201310531391 A CN 201310531391A CN 103551052 B CN103551052 B CN 103551052B
- Authority
- CN
- China
- Prior art keywords
- super
- composite membrane
- hydrophobic
- obtains
- preparation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 239000012528 membrane Substances 0.000 title claims abstract description 27
- 239000002131 composite material Substances 0.000 title claims abstract description 21
- 230000003075 superhydrophobic effect Effects 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 229920002492 poly(sulfone) Polymers 0.000 claims abstract description 30
- 239000004642 Polyimide Substances 0.000 claims abstract description 17
- 229920001721 polyimide Polymers 0.000 claims abstract description 17
- 230000002209 hydrophobic effect Effects 0.000 claims abstract description 16
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 claims abstract description 15
- 239000000835 fiber Substances 0.000 claims abstract description 15
- 229920001296 polysiloxane Polymers 0.000 claims abstract description 15
- 229920000642 polymer Polymers 0.000 claims abstract description 9
- 238000005470 impregnation Methods 0.000 claims abstract description 5
- 239000000203 mixture Substances 0.000 claims abstract description 5
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 12
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 12
- 238000001291 vacuum drying Methods 0.000 claims description 10
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 6
- 229910021529 ammonia Inorganic materials 0.000 claims description 4
- 230000015572 biosynthetic process Effects 0.000 claims description 4
- 238000002386 leaching Methods 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 238000003912 environmental pollution Methods 0.000 abstract description 2
- 238000001035 drying Methods 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Landscapes
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention discloses a kind of preparation method of super-hydrophobic composite membrane, slide lifts out after being immersed in polyimides colloidal sol, and for several times, drying obtains base film layer in repeated impregnations lift; The mixture of dimethyl silicone polymer-g-polysulfones and polysulfone hollow fibre is heated to molten condition and obtains mixed liquor, mixed liquor is put in container; Polymer flow is ejected in container energising, receiver sheet carries out enrichment and obtains hydrophobic layer; Hydrophobic layer is covered on base film layer, obtain super-hydrophobic composite membrane.By the way, the preparation method of super-hydrophobic composite membrane of the present invention, the super-hydrophobic composite membrane obtained combines firmly, there is very strong hydrophobicity, good mechanical property, there is higher porosity and film-strength, whole safe preparation process performance is good, environmental pollution is little, and operation is simple, can effectively reduce production cost.
Description
Technical field
The present invention relates to technical field of membrane, particularly relate to a kind of preparation method of super-hydrophobic 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 recycle utility, effectively can purify again to waste water, 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 be wherein made up of hydrophobic material is hydrophobic film, and the contact angle that fluid drips is formed on film surface is greater than 90 °.The mechanical performance of traditional hydrophobic film is bad, easily ruptures or ftractures, complex manufacturing process during use, and production cost is improved greatly.
Summary of the invention
The technical problem that the present invention mainly solves is to provide a kind of preparation method of super-hydrophobic composite membrane, and the method is safe and reliable, and the film hydrophobic performance obtained is good.
For solving the problems of the technologies described above, the technical scheme that the present invention adopts is: the preparation method providing a kind of super-hydrophobic composite membrane, and comprising step is:
(1) polyimides is dissolved in toluene and also constantly stirs, slow dropping mass percent is the sodium carbonate liquor of 8-10%, and described rate of addition is every 3-4 second one, drips and terminates rear continuations stirring 3-5 hour, dripping ammonia spirit more gradually makes pH value become alkalescence, obtains polyimides colloidal sol;
(2) slide is immersed in the polyimides colloidal sol that step (1) obtains, 10-20 minute is put in leaching, with even speed, slide is lifted out from described polyimides colloidal sol, repeated impregnations lift for several times, to take out after described slide in vacuum drying chamber, the temperature of described vacuum drying chamber is set to 80-100 DEG C, 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, puts in container by described mixed liquor;
(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-hydrophobic 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 of vacuum drying chamber is set to 95 DEG C.
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-hydrophobic composite membrane of the present invention, the super-hydrophobic composite membrane obtained combines firmly, 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.
Detailed description of the invention
Be clearly and completely described to the technical scheme in the embodiment of the present invention below, obviously, described embodiment is only a part of embodiment of the present invention, instead of whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art, not making other embodiments all obtained under creative work prerequisite, belong to the scope of protection of the invention.
Embodiment one:
There is provided a kind of preparation method of super-hydrophobic composite membrane, comprising step is:
(1) polyimides is dissolved in toluene and also constantly stirs, slow dropping mass percent is the sodium carbonate liquor of 9%, and described rate of addition is every 4 second one, drips and terminates rear continuation stirring 4 hours, dripping ammonia spirit more gradually makes pH value become alkalescence, obtains polyimides colloidal sol;
(2) slide is immersed in the polyimides colloidal sol that step (1) obtains, leaching puts 15 minutes, with even speed, slide is lifted out from described polyimides colloidal sol, repeated impregnations lift for several times, to take out after described slide in vacuum drying chamber, the temperature of described vacuum drying chamber is set to 95 DEG C, 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, puts in container by described mixed liquor;
(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-hydrophobic composite membrane.
Embodiment two:
There is provided a kind of preparation method of super-hydrophobic composite membrane, comprising step is:
(1) polyimides is dissolved in toluene and also constantly stirs, slow dropping mass percent is the sodium carbonate liquor of 8%, and described rate of addition is every 3 second one, drips and terminates rear continuation stirring 5 hours, dripping ammonia spirit more gradually makes pH value become alkalescence, obtains polyimides colloidal sol;
(2) slide is immersed in the polyimides colloidal sol that step (1) obtains, leaching puts 17 minutes, with even speed, slide is lifted out from described polyimides colloidal sol, repeated impregnations lift for several times, to take out after described slide in vacuum drying chamber, the temperature of described vacuum drying chamber is set to 88 DEG C, 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, puts in container by described mixed liquor;
(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-hydrophobic composite membrane.
The foregoing is only embodiments of the invention; not thereby the scope of the claims of the present invention is limited; every utilize description of the present invention to do equivalent structure or equivalent flow process conversion; 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-hydrophobic composite membrane, is characterized in that, comprises step to be:
(1) polyimides is dissolved in toluene and also constantly stirs, slow dropping mass percent is the sodium carbonate liquor of 8-10%, and described rate of addition is every 3-4 second one, drips and terminates rear continuations stirring 3-5 hour, dripping ammonia spirit more gradually makes pH value become alkalescence, obtains polyimides colloidal sol;
(2) slide is immersed in the polyimides colloidal sol that step (1) obtains, 10-20 minute is put in leaching, with even speed, slide is lifted out from described polyimides colloidal sol, repeated impregnations lift for several times, to take out after described slide in vacuum drying chamber, the temperature of described vacuum drying chamber is set to 80-100 DEG C, 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, puts in container by described mixed liquor;
(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-hydrophobic composite membrane.
2. the preparation method of super-hydrophobic 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-hydrophobic composite membrane according to claim 1, is characterized in that, described in step (2), the temperature of vacuum drying chamber is set to 95 DEG C.
4. the preparation method of super-hydrophobic 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.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310531391.5A CN103551052B (en) | 2013-11-01 | 2013-11-01 | A kind of preparation method of super-hydrophobic composite membrane |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310531391.5A CN103551052B (en) | 2013-11-01 | 2013-11-01 | A kind of preparation method of super-hydrophobic composite membrane |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103551052A CN103551052A (en) | 2014-02-05 |
| CN103551052B true CN103551052B (en) | 2015-07-29 |
Family
ID=50005514
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310531391.5A Active CN103551052B (en) | 2013-11-01 | 2013-11-01 | A kind of preparation method of super-hydrophobic composite membrane |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103551052B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104307387B (en) * | 2014-10-11 | 2017-08-08 | 南京九思高科技有限公司 | A kind of Kynoar hexafluoropropene super-hydrophobic composite film and preparation method thereof |
| CN109295717B (en) * | 2018-07-31 | 2021-04-27 | 广州中国科学院先进技术研究所 | A kind of method for rapidly preparing oleophobic and hydrophobic membrane |
Citations (3)
| 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 - |
| CN102294182A (en) * | 2011-07-18 | 2011-12-28 | 清华大学 | Preparation method of hydrophobic nano mesoporous molecular sieve filling PDMC composite film |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8622223B2 (en) * | 2008-12-17 | 2014-01-07 | General Electric Company | Membrane assemblies and methods of making and using the same |
| US8597518B2 (en) * | 2009-08-19 | 2013-12-03 | The University Of Connecticut | Pervaporation composite membrane for aqueous solution separation and methods for using the same |
| JP6222625B2 (en) * | 2012-02-16 | 2017-11-01 | 富士フイルム株式会社 | Composite separation membrane and separation membrane module using the same |
-
2013
- 2013-11-01 CN CN201310531391.5A patent/CN103551052B/en active Active
Patent Citations (3)
| 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 - |
| CN102294182A (en) * | 2011-07-18 | 2011-12-28 | 清华大学 | Preparation method of hydrophobic nano mesoporous molecular sieve filling PDMC composite film |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103551052A (en) | 2014-02-05 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101445396B (en) | Method for preparing porcelain insulator surface super-hydrophobic coating | |
| CN103952912B (en) | Wash fast super-hydrophobic cotton and its preparation method and application | |
| CN113546524B (en) | A kind of preparation method of oil-water separation membrane coated with polyvinyl alcohol hydrogel paint | |
| CN103265714A (en) | Polyvinyl alcohol/graphene oxide composite film preparation method | |
| CN103551052B (en) | A kind of preparation method of super-hydrophobic composite membrane | |
| CN109304088A (en) | A kind of seawater desalination membrane resistant to strong acid and alkali and its preparation method and application | |
| CN103102759A (en) | Water-based glass paint containing modified diatomite and preparation method thereof | |
| CN106268378A (en) | A kind of preparation method of hollow fiber compound nanofiltration membrane | |
| CN102765287A (en) | Water transfer printing preparation process for artificial stone | |
| CN103551053B (en) | A kind of preparation method of hydrophobic composite membrane | |
| CN106007392A (en) | Preparation method of ZnO nano coating glass with hydrophobic property | |
| CN103102766A (en) | High adhesive force water-based glass paint and preparation method thereof | |
| CN103406034A (en) | Preparation method of polyether block amide microporous film for film distillation process | |
| CN104793384A (en) | Ultra-thin liquid crystal display and production method thereof | |
| CN107413208B (en) | A kind of preparation method of highly selective gasoline desulfurizing film | |
| CN105541119A (en) | Method for preparing transparent super-hydrophobic coating with sol-gel method | |
| CN105381764A (en) | Method for preparing polystyrene-polyvinyl alcohol double-layer hollow microspheres | |
| CN107603704B (en) | Water-based release agent for fair-faced concrete and preparation method thereof | |
| CN105293948A (en) | Preparation method for hydrophobic organic-modified silicate thin film with adjustable refractive index and silicate thin film | |
| CN111440578B (en) | Water-treatment epoxy pouring sealant for preventing hollow fiber membrane from discoloring and preparation method thereof | |
| CN202860419U (en) | Device for preparing hollow fiber blend membrane | |
| CN105727764B (en) | Photopolymerization modified polyallylamine solid support film and preparation method thereof | |
| CN108219814B (en) | Carboxyl asphalt and preparation process and application thereof | |
| CN115245741A (en) | A kind of preparation method of polydopamine ceramic composite membrane | |
| CN204936360U (en) | A kind of novel carbon fiber heating film and preparation system thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C41 | Transfer of patent application or patent right or utility model | ||
| TR01 | Transfer of patent right |
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 |