CN104761743A - Simple general preparation method of silicone rubber super-hydrophobic surface - Google Patents
Simple general preparation method of silicone rubber super-hydrophobic surface Download PDFInfo
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Abstract
The invention relates to a simple general preparation method of a silicone rubber super-hydrophobic surface. The preparation method comprises the following steps: 1) configuring a viscous solution from 100 parts by weight of alpha,omega-dihydroxy polydimethylsiloxane, 5-8 parts by weight of a curing agent, 0.2-0.3 part by weight of a catalyst, namely di-n-butyl tin dilaurate and 10-200 parts by weight of a solvent, namely n-hexane, casting on a substrate to form a film with the thickness of 500-2000 mu m; 2) enabling 10-50 parts of powder additives (red copper powder, nickel powder, zinc powder, carbon black, graphite powder, silicon dioxide powder, titanium dioxide, ordinary portland cement powder, gypsum powder, barium titanate powder, polyvinylidene fluoride powder and polyphenylene sulfide powder) to pass through a 200-mesh nylon screen, then uniformly scattering on the surface of the newly made room temperature vulcanized silicone rubber viscous solution; and 3) curing at room temperature for 24h, and then rinsing with a large amount of tap water to remove residual powder on the surface to obtain the rubber super-hydrophobic surface. The method for preparing the super-hydrophobic surface on the silicone rubber substrate provided by the invention is simple and general, is suitable for a variety of raw materials and can be used for manufacturing super-hydrophobic waterproof coatings on the surfaces of a variety of materials such as metal, cement, gypsum and timber.
Description
Technical field
The present invention relates to a kind of preparation method of super hydrophobic surface, particularly relate to a kind of simple general use method preparing super hydrophobic surface on silastic material.
Background technology
Silastic material has good hydrophobic performance, and its surface contact angle is lower than 110 °.The glass used in power industry or ceramic insulation sub-surface easily accumulate filth and pollution flashover accident occur, and silicon rubber insulator has excellent resistance to pollution flashover performance because of its good hydrophobicity and hydrophobic transport property.Silicon rubber insulator contact angle common is not at present higher than 110 ° and roll angle is comparatively large, do not reach super-hydrophobic effect.So-called super hydrophobic surface refers to the solid surface being less than 10 ° higher than roll angle while of 150 ° to the static contact angle of water droplet.At nature, lotus leaf surface is most typical natural super hydrophobic surface.So-called " lotus leaf effect " refers to water droplet and presents at lotus leaf surface spherical and unstable, is easily subject to outside slight effect and is rolled off surface.Surface dirt is taken away by water droplet in the process of rolling, and therefore give lotus leaf surface automatically cleaning ability, the reason that lotus leaf surface " goes out mud and do not contaminate " is namely this.But now widely used usual silicone rubber insulator surface does not have self_cleaning effect, the tumbling action of rainwater can not be utilized to be removed completely by surface filth.If low cost can be adopted, common silicon rubber made super-hydrophobic silicon rubber by simple and easy and general method, so just can give the self-cleaning performance of silicon rubber insulator excellence, greatly improve the ability of silicon rubber insulator antifouling work.
At present, preparation method about super-hydrophobic silicon rubber surface has some bibliographical informations, but what these methods had employs expensive fluorination reagent, some preparation methods are complicated and process is loaded down with trivial details, and what have then needs the expensive processing units of dependence and cannot obtain industrial large-scale application.Such as, in the titanium dioxide/silicon rubber composite material of the preparation such as Ding, to employ silicon fluoride rubber be raw material, its material cost than usual silicone rubber exceed a lot (
j. Mater. Chem.,2011,21,6161).Givenchy etc. use the method for acid etch and surface fluorination to prepare silicon rubber super hydrophobic surface, but the acidity that this process uses etching reagent can cause environmental pollution, and preparation process is loaded down with trivial details, also use expensive fluorination reagent in addition, these are unfavorable for the industrialization (Langmuir of these class methods, 2009,25,6448).Therefore, develop silicon rubber super hydrophobic surface low cost, process preparation method that is simple, highly versatile is the most important condition realizing the application of super-hydrophobic silicon rubber industry.
Summary of the invention
The object of the present invention is to provide a kind of simple general use method preparing super hydrophobic surface on silicon rubber.
The present invention is achieved like this: a kind of simple general use preparation method of silicon rubber super hydrophobic surface, it is characterized in that method steps is: the first step, by 100 weight part α ω – dialkyl polydimethylsiloxanes, 5 ~ 8 weight part solidifying agent, the solvent hexane of 0.2 ~ 0.3 part by weight of catalyst di-n-butyltin dilaurate and 10 ~ 80 parts of weight is configured to viscous solution, becomes the film of 500 ~ 2000 μm of thickness in base material top casting; Second step, by the powder additives of 10 ~ 50 parts (red copper powder, nickel powder, zinc powder, carbon black, Graphite Powder 99, SiO 2 powder, titanium dioxide, ordinary Portland cement powder, terra alba, barium titanate powder, polyvinylidene difluoride (PVDF) powder, polyphenylene sulfide powder) by being evenly scattered in the room temperature vulcanized silicone rubber viscous solution surface of brand-new after 200 order nylon mesh; 3rd step, surface residual powder is removed with a large amount of tap water after 24 hours and is namely obtained rubber super hydrophobic surface by self-vulcanizing.
The viscosity of α , ω – dialkyl polydimethylsiloxane of the present invention is 5000 ~ 10000 cp.
The powder additive particle diameter of use of the present invention is less than 200 orders, can pass through 200 order nylon mesh.
Surface residual powder of the present invention uses test-tube brush repeatedly to wash away in tap water to constant weight and namely obtains silicon rubber super hydrophobic surface.
Accompanying drawing explanation
Fig. 1 is the electron scanning micrograph of the SiO 2 powder used in the present invention.
Fig. 2 is the scanning electron photomicrograph of the silica/silicon rubber composite super hydrophobic surface prepared in the present invention.
Fig. 3 is the static contact angle that the silica/silicon rubber composite surface of preparing in the present invention adopts the test of optical contact angle tester.
Fig. 4 is the roll angle that the silica/silicon rubber composite surface of preparing in the present invention adopts the test of optical contact angle tester.
Embodiment
The present invention is described in further detail for embodiment and accompanying drawing below.
Embodiment 1
Be the α , ω – dialkyl polydimethylsiloxane of 5000 cp by 20 g viscosity, 0.5 g solidifying agent tetraethoxysilane and 0.05 g catalyst dibutyltin cinnamic acid di-n-butyl tin are at room temperature dissolved in 100 mL normal hexanes, obtain silicone rubber solution.Then solution is poured over stainless steel substrate surface, glass stick is used to be launched into the shape of 5 cm × 5 cm, the SiO 2 powder after nature levelling by 10 g median sizes being 1-2 micron is surperficial at silicone rubber solution by uniformly dispersing after 200 order nylon mesh, after at room temperature solidifying 24 h subsequently.Finally repeatedly scrub sample surfaces with test-tube brush and tap water, namely obtain silica modified silicon rubber super hydrophobic surface.Use optical contact angle tester to detect (Germany, KRUSS, DSA100), the static contact angle of 5 μ L deionized waters on this surface is 163.6 °, and roll angle is 4.3 °.
Embodiment 2
Be the α , ω – dialkyl polydimethylsiloxane of 5000 cp by 20 g viscosity, 0.5 g solidifying agent tetraethoxysilane and 0.05 g catalyst dibutyltin cinnamic acid di-n-butyl tin are at room temperature dissolved in 100 mL normal hexanes, obtain silicone rubber solution.Then solution is poured over glass sheet surface, glass stick is used to be launched into the shape of 5 cm × 5 cm, the red copper powder powder after nature levelling by 20 g median sizes being 0.5-2 micron is surperficial at silicone rubber solution by uniformly dispersing after 200 order nylon mesh, after at room temperature solidifying 24 h subsequently.Finally repeatedly scrub sample surfaces with test-tube brush and tap water, namely obtain the silicon rubber super hydrophobic surface of copper powder modification.Use optical contact angle tester to detect (Germany, KRUSS, DSA100), the static contact angle of 5 μ L deionized waters on this surface is 165.4 °, and roll angle is 4.7 °.
Embodiment 3
Be the α , ω – dialkyl polydimethylsiloxane of 5000 cp by 20 g viscosity, 0.5 g solidifying agent tetraethoxysilane and 0.05 g catalyst dibutyltin cinnamic acid di-n-butyl tin are at room temperature dissolved in 100 mL normal hexanes, obtain silicone rubber solution.Then solution is poured over board surface, glass stick is used to be launched into the shape of 5 cm × 5 cm, the carbon black powder after nature levelling by 10 g median sizes being 50 nanometers is surperficial at silicone rubber solution by uniformly dispersing after 200 order nylon mesh, after at room temperature solidifying 24 h subsequently.Finally repeatedly scrub sample surfaces with test-tube brush and tap water, namely obtain carbon black modified silicon rubber super hydrophobic surface.Use optical contact angle tester to detect (Germany, KRUSS, DSA100), the static contact angle of 5 μ L deionized waters on this surface is 168.6 °, and roll angle is 3.3 °.
Embodiment 4
Be the α , ω – dialkyl polydimethylsiloxane of 5000 cp by 20 g viscosity, 0.5 g solidifying agent tetraethoxysilane and 0.05 g catalyst dibutyltin cinnamic acid di-n-butyl tin are at room temperature dissolved in 100 mL normal hexanes, obtain silicone rubber solution.Then solution is poured over gypsum board surface, glass stick is used to be launched into the shape of 5 cm × 5 cm, the ordinary Portland cement powder after nature levelling by 15 g median sizes being 1 micron is surperficial at silicone rubber solution by uniformly dispersing after 200 order nylon mesh, after at room temperature solidifying 24 h subsequently.Finally repeatedly scrub sample surfaces with test-tube brush and tap water, namely obtain the silicon rubber super hydrophobic surface of ordinary Portland cement powder modification.Use optical contact angle tester to detect (Germany, KRUSS, DSA100), the static contact angle of 5 μ L deionized waters on this surface is 159.5 °, and roll angle is 6.3 °.
Embodiment 5
Be the α , ω – dialkyl polydimethylsiloxane of 5000 cp by 20 g viscosity, 0.5 g solidifying agent tetraethoxysilane and 0.05 g catalyst dibutyltin cinnamic acid di-n-butyl tin are at room temperature dissolved in 100 mL normal hexanes, obtain silicone rubber solution.Then solution is poured over glass sheet surface, glass stick is used to be launched into the shape of 5 cm × 5 cm, the polyvinylidene difluoride (PVDF) powder after nature levelling by 15 g median sizes being 15 microns is surperficial at silicone rubber solution by uniformly dispersing after 200 order nylon mesh, after at room temperature solidifying 24 h subsequently.Finally repeatedly scrub sample surfaces with test-tube brush and tap water, namely obtain the silicon rubber super hydrophobic surface of polyvinylidene difluoride (PVDF) powder modification.Use optical contact angle tester to detect (Germany, KRUSS, DSA100), the static contact angle of 5 μ L deionized waters on this surface is 159.5 °, and roll angle is 6.3 °.
Embodiment 6
Be the α , ω – dialkyl polydimethylsiloxane of 5000 cp by 10 g viscosity, 0.5 g solidifying agent tetraethoxysilane and 0.05 g catalyst dibutyltin cinnamic acid di-n-butyl tin are at room temperature dissolved in 200 mL normal hexanes, obtain silicone rubber solution.Then solution is poured over stainless steel substrate surface, glass stick is used to be launched into the shape of 5 cm × 5 cm, the barium titanate powder after nature levelling by 15 g median sizes being 1 micron is surperficial at silicone rubber solution by uniformly dispersing after 200 order nylon mesh, after at room temperature solidifying 24 h subsequently.Finally repeatedly scrub sample surfaces with test-tube brush and tap water, namely obtain the silicon rubber super hydrophobic surface of barium titanate powder modification.Use optical contact angle tester to detect (Germany, KRUSS, DSA100), the static contact angle of 5 μ L deionized waters on this surface is 161.3 °, and roll angle is 5.7 °.
Claims (5)
1. the simple general use preparation method of a silicon rubber super hydrophobic surface, it is characterized in that method steps is: the first step, by 100 weight part α ω – dialkyl polydimethylsiloxanes, 5 ~ 8 weight part solidifying agent, the solvent hexane of 0.2 ~ 0.3 part by weight of catalyst di-n-butyltin dilaurate and 10 ~ 80 parts of weight is configured to viscous solution, becomes the film of 500 ~ 2000 μm of thickness in base material top casting; Second step, by the powder additive of 10 ~ 50 parts by being evenly scattered in the room temperature vulcanized silicone rubber viscous solution surface of brand-new after 200 order nylon mesh; 3rd step, surface residual powder is removed with a large amount of tap water after 24 hours and is namely obtained rubber super hydrophobic surface by self-vulcanizing.
2. the simple general use preparation method of a kind of silicon rubber super hydrophobic surface as claimed in claim 1, is peculiarly being: described powder additive is red copper powder, nickel powder, zinc powder, carbon black, Graphite Powder 99, SiO 2 powder, titanium dioxide, ordinary Portland cement powder, terra alba, barium titanate powder, polyvinylidene difluoride (PVDF) powder, polyphenylene sulfide powder.
3. the simple general use preparation method of a kind of silicon rubber super hydrophobic surface as claimed in claim 1, is characterized in that: the viscosity of described α , ω – dialkyl polydimethylsiloxane is 5000 ~ 10000 cp.
4. the simple general use preparation method of a kind of silicon rubber super hydrophobic surface as claimed in claim 1, is characterized in that: the powder additive particle diameter used is less than 200 orders, can pass through 200 order nylon mesh.
5. the simple general use preparation method of a kind of silicon rubber super hydrophobic surface as claimed in claim 1, is characterized in that: surface residual powder uses test-tube brush repeatedly to wash away in tap water to constant weight and namely obtains silicon rubber super hydrophobic surface.
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Cited By (6)
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CN105778137A (en) * | 2016-03-11 | 2016-07-20 | 南昌航空大学 | Preparation method of silicone rubber-based superhydrophobic coating with noctilucent function |
CN106752133A (en) * | 2016-12-07 | 2017-05-31 | 上海交通大学 | The super-hydrophobic coat prepared using Graphene three-dimensional aggregates and its synthetic method and application |
CN109385208A (en) * | 2018-09-12 | 2019-02-26 | 安徽康瑞高科新材料技术工程有限公司 | A kind of insulator antiicing coating and preparation method thereof |
CN109735114A (en) * | 2019-01-09 | 2019-05-10 | 华南理工大学 | Seal ring for drum-type washing silicon rubber nano composite material and preparation method thereof |
CN114752236A (en) * | 2022-04-19 | 2022-07-15 | 苏州大学 | High-reflection wear-resistant super-hydrophobic coating and preparation method thereof |
CN115584656A (en) * | 2022-10-21 | 2023-01-10 | 华南理工大学 | Super-hydrophobic material with photo-thermal effect and preparation method and application thereof |
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CN101497754A (en) * | 2008-01-29 | 2009-08-05 | 罗门哈斯公司 | Acrylic coating powders comprising hydrophobic particles and powder coatings therefrom |
CN103214690A (en) * | 2013-03-22 | 2013-07-24 | 哈尔滨工业大学 | Method for preparing durable super-hydrophobic material |
CN104448374A (en) * | 2014-12-03 | 2015-03-25 | 南昌航空大学 | Preparation method of super-hydrophobic surface of room temperature vulcanized silicone rubber |
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2015
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CN101497754A (en) * | 2008-01-29 | 2009-08-05 | 罗门哈斯公司 | Acrylic coating powders comprising hydrophobic particles and powder coatings therefrom |
CN101481081A (en) * | 2009-01-21 | 2009-07-15 | 重庆大学 | Preparation of composite structure super-hydrophobic film |
CN103214690A (en) * | 2013-03-22 | 2013-07-24 | 哈尔滨工业大学 | Method for preparing durable super-hydrophobic material |
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Cited By (10)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105778137A (en) * | 2016-03-11 | 2016-07-20 | 南昌航空大学 | Preparation method of silicone rubber-based superhydrophobic coating with noctilucent function |
CN106752133A (en) * | 2016-12-07 | 2017-05-31 | 上海交通大学 | The super-hydrophobic coat prepared using Graphene three-dimensional aggregates and its synthetic method and application |
CN106752133B (en) * | 2016-12-07 | 2019-03-29 | 上海交通大学 | Utilize the super-hydrophobic coat and its synthetic method of the preparation of graphene three-dimensional aggregates and application |
CN109385208A (en) * | 2018-09-12 | 2019-02-26 | 安徽康瑞高科新材料技术工程有限公司 | A kind of insulator antiicing coating and preparation method thereof |
CN109735114A (en) * | 2019-01-09 | 2019-05-10 | 华南理工大学 | Seal ring for drum-type washing silicon rubber nano composite material and preparation method thereof |
CN109735114B (en) * | 2019-01-09 | 2020-07-28 | 华南理工大学 | Silicone rubber nano composite material for door sealing ring of drum washing machine and preparation method thereof |
CN114752236A (en) * | 2022-04-19 | 2022-07-15 | 苏州大学 | High-reflection wear-resistant super-hydrophobic coating and preparation method thereof |
CN114752236B (en) * | 2022-04-19 | 2022-12-20 | 苏州大学 | High-reflection wear-resistant super-hydrophobic coating and preparation method thereof |
CN115584656A (en) * | 2022-10-21 | 2023-01-10 | 华南理工大学 | Super-hydrophobic material with photo-thermal effect and preparation method and application thereof |
CN115584656B (en) * | 2022-10-21 | 2024-03-29 | 华南理工大学 | Super-hydrophobic material with photo-thermal effect and preparation method and application thereof |
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