CN104497725A - Preparation methods of superhydrophobic polystyrene (PS)/ZnO composite sol and composite coating - Google Patents
Preparation methods of superhydrophobic polystyrene (PS)/ZnO composite sol and composite coating Download PDFInfo
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- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
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- C08K3/00—Use of inorganic substances as compounding ingredients
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- C08K3/20—Oxides; Hydroxides
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- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
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- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/04—Compounds of zinc
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
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Abstract
The invention provides a preparation method of superhydrophobic polystyrene (PS)/ZnO composite sol. The preparation method comprises the following steps of (1) preparing ZnO particles; (2) carrying out surface modification on the ZnO particles; (3) preparing a superhydrophobic coating, namely adding 3 parts of PS into tetrahydrofuran in a normal temperature state, and sufficiently dissolving PS under the ultrasonic action; adding a proper amount of deionized water, a catalyst and a dispersing agent into a beaker, rapidly stirring for 3 hours under the ultrasonic action, adding 7g of modified ZnO into the solution, and continuing to stir for 5 hours; and then, slowly adding 3g of a PS emulsion and a curing agent into the solution, and magnetically stirring for 4-5 hours under the conditions that the temperature is 40 DEG C and the pH value is equal to 5 to obtain emulsive uniform superhydrophobic PS/ZnO composite sol. The invention also provides a preparation method of a superhydrophobic PS/ZnO composite coating. The contact angle between the superhydrophobic composite coating provided by the invention and water is 156 DEG, the rolling angle of the superhydrophobic composite coating is 8 DEG, and the hydrophobic effect is good. The favorable anticorrosion and oil-water separation effects are achieved.
Description
Technical field
The present invention relates to the preparation method of polystyrene/zinc oxide super-hydrophobic complex sol and compound coating.
Background technology
Body surface has automatically cleaning and anti-corrosion function is nanosecond science and technology age study problem the most widely, it is the target that people pursue that process differing materials surface makes it have ultra-hydrophobicity, as: people the accessory such as shoes, clothes worn do not get wet, the antifogging self-cleaning of kitchen tile and bathroom glass, the hydrophobic preservative property of building external paint and water pipe inwall.
Super-hydrophobic composite material surface, because have excellent hydrophobic ability and good antiseptic property, has a wide range of applications in industry and life.In recent years, find that a kind of preparation technology is simple, with low cost, method environmental protection, stable performance and the antifouling anticorrosion super-hydrophobic coat had both be current developing direction.
Summary of the invention
The invention provides the preparation method of a kind of polystyrene/zinc oxide super-hydrophobic complex sol and compound coating.
The invention provides the preparation method of polystyrene/zinc oxide super-hydrophobic complex sol, step is as follows:
(1) preparation of ZnO particle
(2) modification of ZnO particle surface
10 mass parts ZnO particles to be dissolved in ethanol and deionized water magnetic agitation even, then 0.9 mass parts ten difluoro heptyl propyl trimethoxy silicane is added wherein fully to mix, and by the suspension of mixing 70 DEG C, pH=5 condition stirs 6h; Finally, under 100 DEG C of conditions, modified ZnO is dried, grind for subsequent use;
(3) preparation of super-hydrophobic coat
In normal temperature state, 3 mass parts polystyrene are put into tetrahydrofuran (THF), ultrasonic lower abundant dissolving; Appropriate deionized water, catalyzer, dispersion agent being added in beaker, at ultrasonic lower rapid stirring 3h, then adding wherein through modified 7g ZnO, continuing to stir 5h; Slowly add 3g PS emulsion and solidifying agent wherein again, at 40 DEG C, pH=5 condition lower magnetic force stirring 4-5h, thus obtain the PS/ZnO complex sol of milky homogeneous.
Preferably, the preparation of described ZnO particle is dissolved in deionized water 20 mass parts sodium hydroxide and 20 mass parts zinc chloride, and stir 12h at 60 DEG C of lower magnetic forces, the product obtained is filtered by centrifuge, then clean respectively with dehydrated alcohol and deionized water, and at 600 DEG C after roasting 3h, cooling grinding, thus obtain the ZnO powder product of micro-/ nano hierarchy.
The present invention also provides the preparation method of polystyrene/zinc oxide super-hydrophobic compound coating, after matrix is cleaned up, in the PS/ZnO complex sol that immersion claim 1 or 2 prepares, adopt dip-coating method at matrix surface plated film, after the sample after lift at normal temperatures dry 20 ~ 30 min, the full cross-linked solidification of compound coating is baked to, obtained PS/ZnO super hydrophobic composite coating at 160 DEG C.
Surface energy and the wetting property of surface geometry configuration on solid surface of solid have larger impact, so reduce the chemical energy of solid surface and the micro/nano structure of structure water repellent surface, are the infiltrating main method of research solid surface.Because ZnO particle surface energy is higher, easily form irregular aggregate and agglomerate, and DFTMS comprises a large amount of-CF
2-hydrophobic group, end contains-CH
3hydrophobic group, therefore has lower surface energy through the ZnO particle that DFTMS is modified.When ZnO particle is immersed in DFTMS solution ,-OH the Interaction of substituents in a large amount of-OH group of particle surface and DFTMS, the condensation reaction that is hydrolyzed forms hydrophobic particle.
PS is a kind of easy machine-shaping and nontoxic cheap thermoplastic resin, with DFTMS as bridge grafting low-surface energy substance PS on ZnO particle, the two be combined with each other, and can effectively reduce inorganic and difference that is organic interface, strengthens the mutual solubility having inorganic phase and organic phase.
The contact angle of super hydrophobic composite coating of the present invention and water is 156 °, and roll angle is 8 °, presents good hydrophobic effect.Meanwhile, there is the effect of good preservative activity and oily water separation.
Embodiment
Following embodiment is convenient to understand the present invention better, but does not limit the present invention.Experimental technique in following embodiment, if no special instructions, is ordinary method.
embodiment 1
(1) preparation of ZnO particle
By 20g sodium hydroxide (NaOH) and 20g zinc chloride (ZnCl
2) be dissolved in certain deionized water, and stir 12h at 60 DEG C of lower magnetic forces, the product obtained is filtered by centrifuge, then twice is cleaned respectively with dehydrated alcohol and deionized water, and to be put in muffle furnace at 600 DEG C after roasting 3h, cooling grinding, thus obtain the ZnO powder product of micro-/ nano hierarchy.The ZnO product purity obtained is higher, and crystal property is better, and particle size range is between 255 ~ 615 nm.
(2) modification of ZnO particle surface
By hydrothermal reaction process, modification is carried out to ZnO particle surface, 10g ZnO particle is dissolved in magnetic agitation in ethanol and deionized water even, again 0.9g ten difluoro heptyl propyl trimethoxy silicane (DFTMS) is added and wherein fully mix, and by the suspension of mixing at 70 DEG C, pH=5 condition stirring 6h.Finally, under 100 DEG C of conditions, modified ZnO is dried, grind for subsequent use.
Untreated ZnO particle has very strong wetting ability, and ZnO particle at Free-rolling above, can show good hydrophobic performance through modified water droplet.
(3) preparation of super-hydrophobic coat
In normal temperature state, 3g polystyrene (PS) is put into tetrahydrofuran (THF), ultrasonic lower abundant dissolving is stand-by.Appropriate deionized water, catalyzer (ammoniacal liquor), dispersion agent (sodium laurylsulfonate) being added in beaker, at ultrasonic lower rapid stirring 3h, then adding wherein through modified 7g ZnO, continuing to stir 5h.Slowly add 3g PS emulsion and solidifying agent (KH-550) more wherein, at 40 DEG C, pH=5 condition lower magnetic force stirring 4-5h, thus obtain the PS/ZnO complex sol of milky homogeneous.
Finally, stand-by after steel matrix surface treatment is clean, immerse subsequently in PS/ZnO complex sol, adopt dip-coating method at steel matrix surface coating.By repetitive operation for several times, after the sample after lift at normal temperatures dry 20 ~ 30 min, the full cross-linked solidification of compound coating is baked at 160 DEG C, obtained PS/ZnO super hydrophobic composite coating.
Performance test:
(1) ZnO coatingsurface uniform ground, compactness is good, is about 0 ° with the contact angle of water.ZnO coating particle diameter through modification becomes large, and surface microscopic configuration expands abundant, and has lower surface energy, is 152 ° with the contact angle of water.Modification-ZnO/PS compound coating roughness and porosity all increase, present the dual coarse structure of micro-/ nano, can effectively reduce the contact area between coating and water droplet, the contact angle of compound coating and water is 156 °, roll angle is 8 °, presents good hydrophobic effect.
(2) when compound coating thermal treatment temp is at 160 DEG C, the static contact angle of water and water-intake rate are respectively 156 ° and 7.3%, and coating hydrophobic effect is best; When thermal treatment temp is lower than 160 DEG C, hydrophobic effect and water-intake rate are not good, and this is caused by thermoplastic resin not exclusively solidifies; When thermal treatment temp increases to 180 DEG C, coating contact angle slightly declines, and water-intake rate increases, and this may be that coating surface structure ftractures, and organo-functional group has certain decomposition, thus affects the hydrophobicity of coating because coating curing temperatures is too high.
(3), after naked steel, PS film, PS/ZnO film being soaked 36h in the NaCl solution of 3%, three-electrode system test electrochemical tests and ac impedance spectroscopy is adopted.Result shows, and after steel surface applies PS film and PS/ZnO composite membrane, corrosion resistance nature is all significantly improved, and corrosion potential is just moving to-624 mV and-586 mV by-890 mV of naked steel, and corrosion electric current density has significant decline, is 2.8 × 10
-7a/cm
2, because polystyrene is polymer amorphous polymer, himself close structure is connected and does not seamlessly absorb water, and anti-permeability and exhibit excellent moisture barrier properties, show good Corrosion Protection.PS/ZnO film to be shuffled about 38 mV compared with the corrosion potential of PS film, corrosion current slightly declines, compelx coating surface does not have bubble obscission, compactness and the homogeneity of compelx coating improve, show good bonding force between metallic matrix and compelx coating, preservative effect is further improved.
(4) the PS/ZnO complex sol prepared is coated on cotton textiles, dries stand-by in atmosphere.Result shows: the contact angle of water droplet on cotton fabric is 158 °, shows good ultra-hydrophobicity.Using the filter paper of cotton superhydrophobic coating as funnel, and 40 mL oil and 40 mL water are mixed in beaker, beaker concussion are mixed, mixed solution is poured in funnel and start to be separated gradually, until flow down from funnel without obvious drop.Finally, the You Heshui after being separated is respectively charged into two graduated cylinders, as the more known oily water separation rate of figure is about 86%.After cotton fabric applies PS/ZnO super hydrophobic composite coating, coating immerses in cotton fabric, and embed parcel fiber surface and form the coarse composite structure of micro-/ nano, it is loose porous that surface tissue becomes, and specific surface area diminishes.Exactly because have this structure, make oil to filter cotton fabric, and water is effectively blocked on cotton fabric, reaches the effect of oily water separation.
Last it is noted that the foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, although with reference to previous embodiment to invention has been detailed description, for a person skilled in the art, it still can be modified to the technical scheme described in foregoing embodiments, or carries out equivalent replacement to wherein portion of techniques feature.Within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (3)
1. the preparation method of polystyrene/zinc oxide super-hydrophobic complex sol, is characterized in that: step is as follows:
(1) preparation of ZnO particle
(2) modification of ZnO particle surface
10 mass parts ZnO particles to be dissolved in ethanol and deionized water magnetic agitation even, then 0.9 mass parts ten difluoro heptyl propyl trimethoxy silicane is added wherein fully to mix, and by the suspension of mixing 70 DEG C, pH=5 condition stirs 6h; Finally, under 100 DEG C of conditions, modified ZnO is dried, grind for subsequent use;
(3) preparation of super-hydrophobic coat
In normal temperature state, 3 mass parts polystyrene are put into tetrahydrofuran (THF), ultrasonic lower abundant dissolving; Appropriate deionized water, catalyzer, dispersion agent being added in beaker, at ultrasonic lower rapid stirring 3h, then adding wherein through modified 7g ZnO, continuing to stir 5h; Slowly add 3g PS emulsion and solidifying agent wherein again, at 40 DEG C, pH=5 condition lower magnetic force stirring 4-5h, thus obtain the PS/ZnO complex sol of milky homogeneous.
2. method according to claim 1, it is characterized in that: the preparation of described ZnO particle is dissolved in deionized water 20 mass parts sodium hydroxide and 20 mass parts zinc chloride, and stir 12h at 60 DEG C of lower magnetic forces, the product obtained is filtered by centrifuge, then clean respectively with dehydrated alcohol and deionized water, and at 600 DEG C after roasting 3h, cooling grinding, thus obtain the ZnO powder product of micro-/ nano hierarchy.
3. the preparation method of polystyrene/zinc oxide super-hydrophobic compound coating, it is characterized in that: be after matrix is cleaned up, in the PS/ZnO complex sol that immersion claim 1 or 2 prepares, adopt dip-coating method at matrix surface plated film, after the sample after lift at normal temperatures dry 20 ~ 30 min, the full cross-linked solidification of compound coating is baked to, obtained PS/ZnO super hydrophobic composite coating at 160 DEG C.
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Cited By (5)
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| CN106479305A (en) * | 2015-08-25 | 2017-03-08 | 石海旺 | A kind of automobile-used water-repelling agent of UV resistant |
| CN109111830A (en) * | 2018-09-02 | 2019-01-01 | 张家港市山牧新材料技术开发有限公司 | A kind of preparation method of zinc oxide-epoxy resin composite coating |
| CN109248570A (en) * | 2018-09-28 | 2019-01-22 | 成都其其小数科技有限公司 | A kind of preparation method of PAN/PAMS/ZnO water-oil separationg film |
| CN112076726A (en) * | 2019-06-12 | 2020-12-15 | 中国石油化工股份有限公司 | Mesoporous molecular sieve loaded with ionic liquid and preparation method and application thereof |
| CN117417667A (en) * | 2023-11-09 | 2024-01-19 | 海南热带海洋学院 | Super-amphiphobic composite coating for marine equipment and preparation method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106479305A (en) * | 2015-08-25 | 2017-03-08 | 石海旺 | A kind of automobile-used water-repelling agent of UV resistant |
| CN109111830A (en) * | 2018-09-02 | 2019-01-01 | 张家港市山牧新材料技术开发有限公司 | A kind of preparation method of zinc oxide-epoxy resin composite coating |
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| CN112076726A (en) * | 2019-06-12 | 2020-12-15 | 中国石油化工股份有限公司 | Mesoporous molecular sieve loaded with ionic liquid and preparation method and application thereof |
| CN117417667A (en) * | 2023-11-09 | 2024-01-19 | 海南热带海洋学院 | Super-amphiphobic composite coating for marine equipment and preparation method thereof |
| CN117417667B (en) * | 2023-11-09 | 2024-07-02 | 海南热带海洋学院 | Super-amphiphobic composite coating for marine equipment and preparation method thereof |
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