CN103537199A - Preparation method of hydrophobic composite film - Google Patents
Preparation method of hydrophobic composite film Download PDFInfo
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- CN103537199A CN103537199A CN201310531402.XA CN201310531402A CN103537199A CN 103537199 A CN103537199 A CN 103537199A CN 201310531402 A CN201310531402 A CN 201310531402A CN 103537199 A CN103537199 A CN 103537199A
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- hydrophobic composite
- composite membrane
- alumina plate
- hydrophobic
- composite film
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Abstract
The invention discloses a preparation method of a hydrophobic composite film. The method comprises the following steps: dissolving polyvinylidene fluoride and triethyl phosphate in dimethylacetamide to obtain a casting film liquid, soaking an aluminum oxide plate in the casting film liquid, repeatedly dipping and pulling for many times and drying to obtain the aluminum oxide plate with a base film on the surface; and dissolving tetramethoxysilane, polymethyl methacrylate and fluorosilane in a mixed solvent to obtain a sol, dropping the sol on the aluminum oxide plate with the base film on the surface, and drying the aluminum oxide plate to obtain the hydrophobic composite film. Through the above manner, the preparation method of the hydrophobic composite film disclosed by the invention is simple to operate. The preparation process can be realized with simple instruments. The raw materials are wide in source, so that the production cost of the preparation process can be lowered. The method is applicable to production on a large scale. The hydrophobic composite film obtained by the method is good in performance. The water contact angle of a hydrophobic layer is greater than 160 degrees. Meanwhile, the hydrophobic composite film is excellent in mechanical property.
Description
Technical field
The present invention relates to membrane technology field, particularly relate to a kind of manufacture method of hydrophobic composite membrane.
Background technology
Film is the material with Selective Separation function, and separation, purifying, the concentrated process of utilizing the Selective Separation of film to realize the different component of feed liquid are called membrane separation technique.It is separated that membrane separation technique and traditional filter method different are that film can carry out in molecular range, and membrane separation technique is a kind of physical process, does not need to occur the variation of phase and adds auxiliary agent.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 °.Traditional hydrophobic film mostly needs special process equipment or complicated technical process in manufacture process, can not in large-scale production, apply.
Summary of the invention
The technical problem that the present invention mainly solves is to provide a kind of manufacture method of hydrophobic 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 manufacture method of hydrophobic composite membrane is provided, comprises that step is:
(1) aluminium sheet is inserted in the mixed solution of sulfuric acid and oxalic acid, and make mixed solution energising 30-40 minute, the phosphoric acid that the chromic acid that is 2-3% by mass percent after taking out and mass percent are 4-7% cleans the aluminium sheet after oxidation, repeating the aluminium sheet of above-mentioned steps after to described oxidation is oxidized for the second time again, be 2-3 hour conduction time, obtains alumina plate after cleaning;
(2) Kynoar and triethyl phosphate are dissolved in middle dimethylacetylamide and constantly and stir and obtain casting solution, the alumina plate obtaining in step (1) is immersed in described casting solution, soak and put 45-50 minute, with even speed, slide is lifted out from described polyimides colloidal sol, repeated impregnations lifts for several times, wherein said pull rate is 10-16cm/min, in temperature, is to dry and obtain the alumina plate that there is base film layer on surface at 80-90 ℃;
(3) tetramethoxy-silicane, polymethyl methacrylate and silicon fluoride are dissolved in mixed solvent, at room temperature stir and within 10-12 hour, obtain colloidal sol, the mass ratio of wherein said tetramethylsilane, described polymethyl methacrylate and described silicon fluoride is 2-4:1:0.5-0.7, colloidal sol is dripped in surface and had on the alumina plate of base film layer, alumina plate is put in vacuum drying chamber dry, obtain hydrophobic composite membrane, the temperature setting of wherein said vacuum drying chamber is set to 120-140 ℃.
In a preferred embodiment of the present invention, described in step (1), the volume ratio of chromic acid and described phosphoric acid is 1:1-3.
In a preferred embodiment of the present invention, described in step (2), pull rate is 13cm/min, and bake out temperature is 88 ℃.
In a preferred embodiment of the present invention, described in step (3), the mass ratio of tetramethylsilane, described polymethyl methacrylate and described silicon fluoride is 3:1:0.6.
The invention has the beneficial effects as follows: the manufacture method of hydrophobic composite membrane of the present invention, the method is simple to operate, need simple instrument can complete manufacture process, raw material sources are extensive, can reduce the production cost of manufacture process, suitable large-scale production, the hydrophobic composite membrane hydrophobic performance obtaining is good, the water contact angle of this hydrophobic layer can be greater than 160 °, and mechanical performance is excellent simultaneously.
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 manufacture method of hydrophobic composite membrane is provided, comprises that step is:
(1) aluminium sheet is inserted in the mixed solution of sulfuric acid and oxalic acid, and make mixed solution energising 30-40 minute, the phosphoric acid that the chromic acid that is 3% by mass percent after taking out and mass percent are 5% cleans the aluminium sheet after oxidation, the volume ratio of wherein said chromic acid and described phosphoric acid is 1:1, repeating the aluminium sheet of above-mentioned steps after to described oxidation is oxidized for the second time again, be 2 hours conduction time, obtains alumina plate after cleaning;
(2) Kynoar and triethyl phosphate are dissolved in middle dimethylacetylamide and constantly and stir and obtain casting solution, the alumina plate obtaining in step (1) is immersed in described casting solution, soak and put 47 minutes, with even speed, slide is lifted out from described polyimides colloidal sol, repeated impregnations lifts for several times, wherein said pull rate is 13cm/min, in temperature, is to dry and obtain the alumina plate that there is base film layer on surface at 88 ℃;
(3) tetramethoxy-silicane, polymethyl methacrylate and silicon fluoride are dissolved in mixed solvent, at room temperature stir and within 12 hours, obtain colloidal sol, the mass ratio of wherein said tetramethylsilane, described polymethyl methacrylate and described silicon fluoride is 3:1:0.6, colloidal sol is dripped in surface and had on the alumina plate of base film layer, alumina plate is put in vacuum drying chamber dry, obtain hydrophobic composite membrane, the temperature setting of wherein said vacuum drying chamber is set to 135 ℃.
Embodiment bis-:
A kind of manufacture method of hydrophobic composite membrane is provided, comprises that step is:
(1) aluminium sheet is inserted in the mixed solution of sulfuric acid and oxalic acid, and make mixed solution energising 30-40 minute, the phosphoric acid that the chromic acid that is 2% by mass percent after taking out and mass percent are 7% cleans the aluminium sheet after oxidation, the volume ratio of wherein said chromic acid and described phosphoric acid is 1:2, repeating the aluminium sheet of above-mentioned steps after to described oxidation is oxidized for the second time again, be 3 hours conduction time, obtains alumina plate after cleaning;
(2) Kynoar and triethyl phosphate are dissolved in middle dimethylacetylamide and constantly and stir and obtain casting solution, the alumina plate obtaining in step (1) is immersed in described casting solution, soak and put 50 minutes, with even speed, slide is lifted out from described polyimides colloidal sol, repeated impregnations lifts for several times, wherein said pull rate is 15cm/min, in temperature, is to dry and obtain the alumina plate that there is base film layer on surface at 82 ℃;
(3) tetramethoxy-silicane, polymethyl methacrylate and silicon fluoride are dissolved in mixed solvent, at room temperature stir and within 10 hours, obtain colloidal sol, the mass ratio of wherein said tetramethylsilane, described polymethyl methacrylate and described silicon fluoride is 2:1:0.5, colloidal sol is dripped in surface and had on the alumina plate of base film layer, alumina plate is put in vacuum drying chamber dry, obtain hydrophobic composite membrane, the temperature setting of wherein said vacuum drying chamber is set to 125 ℃.
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 manufacture method for hydrophobic composite membrane, is characterized in that, comprises that step is:
(1) aluminium sheet is inserted in the mixed solution of sulfuric acid and oxalic acid, and make mixed solution energising 30-40 minute, the phosphoric acid that the chromic acid that is 2-3% by mass percent after taking out and mass percent are 4-7% cleans the aluminium sheet after oxidation, repeating the aluminium sheet of above-mentioned steps after to described oxidation is oxidized for the second time again, be 2-3 hour conduction time, obtains alumina plate after cleaning;
(2) Kynoar and triethyl phosphate are dissolved in middle dimethylacetylamide and constantly and stir and obtain casting solution, the alumina plate obtaining in step (1) is immersed in described casting solution, soak and put 45-50 minute, with even speed, slide is lifted out from described polyimides colloidal sol, repeated impregnations lifts for several times, wherein said pull rate is 10-16cm/min, in temperature, is to dry and obtain the alumina plate that there is base film layer on surface at 80-90 ℃;
(3) tetramethoxy-silicane, polymethyl methacrylate and silicon fluoride are dissolved in mixed solvent, at room temperature stir and within 10-12 hour, obtain colloidal sol, the mass ratio of wherein said tetramethylsilane, described polymethyl methacrylate and described silicon fluoride is 2-4:1:0.5-0.7, colloidal sol is dripped in surface and had on the alumina plate of base film layer, alumina plate is put in vacuum drying chamber dry, obtain hydrophobic composite membrane, the temperature setting of wherein said vacuum drying chamber is set to 120-140 ℃.
2. the manufacture method of hydrophobic composite membrane according to claim 1, is characterized in that, described in step (1), the volume ratio of chromic acid and described phosphoric acid is 1:1-3.
3. the manufacture method of hydrophobic composite membrane according to claim 1, is characterized in that, described in step (2), pull rate is 13cm/min, and bake out temperature is 88 ℃.
4. the manufacture method of hydrophobic composite membrane according to claim 1, is characterized in that, described in step (3), the mass ratio of tetramethylsilane, described polymethyl methacrylate and described silicon fluoride is 3:1:0.6.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310531402.XA CN103537199A (en) | 2013-11-01 | 2013-11-01 | Preparation method of hydrophobic composite film |
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| CN201310531402.XA CN103537199A (en) | 2013-11-01 | 2013-11-01 | Preparation method of hydrophobic composite film |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104028115A (en) * | 2014-06-03 | 2014-09-10 | 上海应用技术学院 | Carboxylation graphene oxide/polyvinylidene fluoride compiste ultrafiltration membrane and preparation method thereof |
| CN104523371A (en) * | 2015-01-22 | 2015-04-22 | 利洁(福建)卫生用品科技有限公司 | Physiological sanitary towel |
| CN107237141A (en) * | 2017-05-08 | 2017-10-10 | 上海大学 | The preparation method that the hydrophobic polyimides that a kind of surface is modified is weaved cotton cloth |
-
2013
- 2013-11-01 CN CN201310531402.XA patent/CN103537199A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104028115A (en) * | 2014-06-03 | 2014-09-10 | 上海应用技术学院 | Carboxylation graphene oxide/polyvinylidene fluoride compiste ultrafiltration membrane and preparation method thereof |
| CN104523371A (en) * | 2015-01-22 | 2015-04-22 | 利洁(福建)卫生用品科技有限公司 | Physiological sanitary towel |
| CN104523371B (en) * | 2015-01-22 | 2018-11-06 | 黄文鹏 | Sanitary napkin |
| CN107237141A (en) * | 2017-05-08 | 2017-10-10 | 上海大学 | The preparation method that the hydrophobic polyimides that a kind of surface is modified is weaved cotton cloth |
| CN107237141B (en) * | 2017-05-08 | 2019-10-11 | 上海大学 | A kind of preparation method for the hydrophobic polyimides woven fabric that surface is modified |
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Application publication date: 20140129 |