CN104448374A - Preparation method of super-hydrophobic surface of room temperature vulcanized silicone rubber - Google Patents
Preparation method of super-hydrophobic surface of room temperature vulcanized silicone rubber Download PDFInfo
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Abstract
The invention discloses a preparation method of a super-hydrophobic surface of room temperature vulcanized silicone rubber. The preparation method comprises the following steps: (1) preparing 100 parts of alpha, omega-dyhydroxyl polydimethylsiloxane, 4-6 parts of a curing agent tetraethoxysilane, 0.1-0.5 part of a catalyst di-n-butyltin dilaurate and 20-100 parts of a solvent normal hexane into a viscous solution, pouring into a solution film which is 200-500 microns thick on sheet glass and defoaming in vacuum at room temperature; (2) uniformly sieving 5-20 parts of a hydrophobic powder additive on the surface of the viscous solution of room temperature vulcanized silicone rubber which is not cured by virtue of an 80-400-mesh stainless steel sample sieve; and (3) after standing for 24 hours at room temperature, eliminating residual powder on the surface to obtain the super-hydrophobic surface of room temperature vulcanized silicone rubber. The super-hydrophobic surface of room temperature vulcanized silicone rubber disclosed by the invention is simple in preparation method, and the used raw materials are easily available and low in price, so that the super-hydrophobic surface of room temperature vulcanized silicone rubber can be used for surface waterproofness, pollution prevention and self-cleaning of building materials.
Description
Technical field
The present invention relates to a kind of preparation method of super hydrophobic surface, particularly relate to a kind of method preparing super hydrophobic surface on room temperature vulcanized silicone rubber material substrate.
Background technology
Silicon rubber has good high and low temperature resistance, keeps its original intensity and elasticity in the temperature range of subzero 90 DEG C to 250 DEG C.In addition, silicon rubber also has excellent electrical insulating property, oxytolerant resistance to deterioration, fast light resistance to deterioration and mildew resistance, chemical stability etc.Because silastic product has excellent over-all properties, thus oneself electric, electronics, aerospace, automobile, mechanical chemical industry, instrument, etc. industry and health care daily life every field obtain a wide range of applications.But current commercial silicon rubber does not have super-hydrophobicity.
So-called super-hydrophobicity refers to the solid surface static contact angle of water droplet being greater than to 150 °.Water droplet on super hydrophobic surface plays pendulum, be subject to vibration a little that the external world causes (as wind, mechanical vibration etc.) water droplet on super hydrophobic surface all can be made to tumble surface rapidly, thus give the functions such as super hydrophobic surface waterproof, automatically cleaning, antifouling, frost prevention, antifog, ice-covering-proof, protection against corrosion and drag reduction.At nature, many animals and plants all have superhydrophobic characteristic.Wherein most typical example is exactly lotus leaf surface and butterfly's wing.Therefore, super hydrophobic surface has broad application prospects in fields such as building external paint, insulator surface coating, high-tension cable surface, windshields.
Obviously, if give silicon rubber with super-hydrophobicity, by automatically cleaning, antifouling property that acquisition usual silicone rubber material does not have, the extreme water-block energy particularly " dripping and be not stained with ".But silicon rubber super hydrophobic surface will be enable to obtain large-scale application in daily life, and technology of preparing is crucial.At present, about the technology of preparing of super-hydrophobic silicon rubber surface gets a larger development.But these super hydrophobic surface preparation technologies based on silicon rubber are usually very complicated, the technology such as such as micro-nano technology, nanolithographic, electrochemical process, sol-gel method, have that equipment requirements is high, long in time limit, high in cost of production drawback, cause complex steps, big area the shortcoming such as cannot to prepare, seriously constrain the practical application of silicon rubber super hydrophobic surface.Therefore, developing a kind of simple and practical preparation method, is the key promoting super hydrophobic material application.
Summary of the invention
The object of the present invention is to provide a kind of low cost simple preparation method of room temperature vulcanized silicone rubber super hydrophobic surface.
The present invention is achieved like this: a kind of preparation method of room temperature vulcanized silicone rubber super hydrophobic surface, it is characterized in that preparation process comprises three steps:
The first step, by 100 weight part α ω – dialkyl polydimethylsiloxanes, 4 ~ 6 weight part solidifying agent tetraethoxysilanes, the solvent hexane of 0.1 ~ 0.5 part by weight of catalyst di-n-butyltin dilaurate and 20 ~ 100 weight parts is configured to viscous solution, the solution film of 200 ~ 500 μm of thickness is become in sheet glass top casting, and at room temperature vacuum defoamation;
Second step, the drainage powder additive (modification infusorial earth, modified zinc oxide, modifying titanium dioxide, improved silica, modification copper powder, modified aluminium powder and polytetrafluoroethylene powder) of 5 ~ 20 weight parts is evenly sieved by 80 ~ 400 order stainless steel sub-sieves and drops on above-mentioned uncured room temperature vulcanized silicone rubber viscous solution film surface, and make it cover whole surface completely;
3rd step, room temperature leaves standstill after 24 hours and namely the removing of surface residual powder is obtained room temperature vulcanized silicone rubber super hydrophobic surface.
The viscosity of α ， ω – dialkyl polydimethylsiloxane of the present invention is 1000 ~ 20000 cp.
Drainage powder of the present invention is the one in dodecyl triethoxyl silane modification infusorial earth powder, Octadecane base trichlorosilane improved silica powder, the modified oxidized zinc powder of n-dodecyl mereaptan, Octadecane base Trimethoxy silane modified titanium dioxide powder, n-dodecyl mereaptan modification copper powder, dodecyl triethoxyl silane modified aluminium powder and polytetrafluoroethylene powder.
Drainage powder particle diameter of the present invention is 10 nm ~ 20 μm.
Surface residual powder of the present invention uses tap water and test-tube brush repeatedly to wash away to constant weight.
Technique effect of the present invention is: compared with prior art not only technique is simple for the preparation method of room temperature vulcanized silicone rubber super hydrophobic surface of the present invention, with low cost, do not need the equipment of complex and expensive, and polytype drainage powder is suitable for, the range of application of room temperature vulcanized silicone rubber can be expanded.
Accompanying drawing explanation
Fig. 1 is the electron scanning micrograph of the Zinc oxide powder used in the present invention.
The super hydrophobic surface drop shape that in Fig. 2 the present invention, hydrophobic modified zinc oxide room temperature vulcanized silicone rubber obtains, wherein illustration is the static contact angle of optical contact angle tester test.
Embodiment
The present invention is described in further detail for embodiment and accompanying drawing below.
Embodiment 1
Under room temperature, 1 mL n-dodecyl mereaptan is dissolved in 50 ml normal hexanes; Then in this solution, add the Zinc oxide powder that 10 g particle diameters are 200 ~ 400 nm, magnetic agitation forms suspension; After Keep agitation 30 min, by suspension centrifugal analysis, namely solid vacuum-drying is obtained hydrophobic Zinc oxide powder to constant weight.
It is the α ω – dialkyl polydimethylsiloxane of 10000 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 10 mL normal hexanes, obtain room temperature vulcanized silicone rubber precursor solution.Then precursor solution is poured over surface of plate glass, and is launched into the shape of 2 cm × 5 cm with glass stick, at room temperature vacuum defoamation 5 min after natural levelling.The hydrophobic Zinc oxide powder of 3 g is put into 200 order stainless steel sub-sieves, it is evenly sieved and drops on room temperature vulcanized silicone rubber precursor solution surface, after at room temperature solidifying 24 h subsequently.Finally repeatedly scrub sample surfaces with test-tube brush and tap water, remove the hydrophobic oxide powder and zinc adhered to loosely last, namely obtain the room temperature vulcanized silicone rubber super hydrophobic surface of hydrophobic modified zinc oxide.Use optical contact angle tester to detect (Germany, KRUSS, DSA100), the static contact angle of 5 μ L deionized waters on this surface is 165.6 °.
Embodiment 2
Under room temperature, 50 μ L dodecyl triethoxyl silanes are dissolved in 50 ml dehydrated alcohols; Then in this solution, add the diatomite powder that 10 g particle diameters are 10 μm, magnetic agitation forms suspension; After Keep agitation 30 min, by suspension centrifugal analysis, namely solid vacuum-drying is obtained hydrophobic diatomite powder to constant weight.
It is the α ω – dialkyl polydimethylsiloxane of 10000 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 10 mL normal hexanes, obtain room temperature vulcanized silicone rubber precursor solution.Then precursor solution is poured over surface of plate glass, and is launched into the shape of 5 cm × 10 cm with glass stick, at room temperature vacuum defoamation 5 min after natural levelling.The hydrophobic diatomite powder of 5 g is put into 100 order stainless steel sub-sieves, it is evenly sieved and drops on room temperature vulcanized silicone rubber precursor solution surface, after at room temperature solidifying 24 h subsequently.Finally repeatedly scrub sample surfaces with test-tube brush and tap water, remove the hydrophobic diatomite in powder adhered to loosely last, namely obtain the room temperature vulcanized silicone rubber super hydrophobic surface of hydrophobic modified zinc oxide.Optical contact angle tester detects, and the static contact angle of 5 μ L deionized waters on this surface is 161.3 °.
Embodiment 3
Under room temperature, 20 μ L Octadecane base trichlorosilanes are dissolved in 50 ml dehydrated alcohols; Then in this solution, add the silica dioxide granule (Meteorological Act white carbon black, model M5, Shanghai Cabot Chemical Co., Ltd.) that 5 g particle diameters are 12 nm, magnetic agitation forms colloidal sol; By this colloidal sol electric drying oven with forced convection always at 60 DEG C dry 24 h obtain hydrophobic silicon dioxide powder.
It is the α ω – dialkyl polydimethylsiloxane of 5000 cp by 5 g viscosity, 0.25 g solidifying agent tetraethoxysilane and 0.02 g catalyst dibutyltin cinnamic acid di-n-butyl tin are at room temperature dissolved in 5 mL normal hexanes, obtain room temperature vulcanized silicone rubber precursor solution.Then precursor solution is poured over surface of plate glass, and is launched into the shape of 10 cm × 10 cm with glass stick, at room temperature vacuum defoamation 5 min after natural levelling.2 g hydrophobic silica powders are put into 500 order stainless steel sub-sieves, it is evenly sieved and drops on room temperature vulcanized silicone rubber precursor solution surface, after at room temperature solidifying 24 h subsequently.Finally repeatedly scrub sample surfaces with test-tube brush and tap water, after removing the hydrophobic silica powder adhered to loosely, namely obtain the room temperature vulcanized silicone rubber super hydrophobic surface of hydrophobic titanium dioxide Si modification.Optical contact angle tester detects, and the static contact angle of 5 μ L deionized waters on this surface is 161.3 °.
Embodiment 4
Under room temperature, 30 μ L Octadecane base trimethoxy silicon are dissolved in 50 ml dehydrated alcohols; Then in this solution, add the titania powder (Shanghai ultra micro nano material company limited) that 6 g particle diameters are 80 nm
Meteorological Act white carbon black, model M5, Shanghai Cabot Chemical Co., Ltd.), magnetic agitation forms suspension; After Keep agitation 30 min, by suspension centrifugal analysis, namely solid vacuum-drying is obtained hydrophobic titanium dioxide dust end to constant weight.
It is the α ω – dialkyl polydimethylsiloxane of 20000 cp by 5 g viscosity, 0.25 g solidifying agent tetraethoxysilane and 0.02 g catalyst dibutyltin cinnamic acid di-n-butyl tin are at room temperature dissolved in 50 mL normal hexanes, obtain room temperature vulcanized silicone rubber precursor solution.Then precursor solution is poured over surface of plate glass, and is launched into the shape of 10 cm × 10 cm with glass stick, at room temperature vacuum defoamation 5 min after natural levelling.200 order stainless steel sub-sieves are put at 5 g hydrophobic titanium dioxide dust ends, it is evenly sieved and drops on room temperature vulcanized silicone rubber precursor solution surface, after at room temperature solidifying 24 h subsequently.Finally repeatedly scrub sample surfaces with test-tube brush and tap water, remove the hydrophobic titanium dioxide dust adhered to loosely last, namely obtain the room temperature vulcanized silicone rubber super hydrophobic surface of hydrophobic titanium dioxide modification.Optical contact angle tester detects, and the static contact angle of 5 μ L deionized waters on this surface is 157.4 °.
Embodiment 5
Under room temperature, 2 mL n-dodecyl mereaptan are dissolved in 50 ml dehydrated alcohols; Then in this solution, add 20 g particle diameters be less than 300 object copper powders (paddy field, Shanghai material Science and Technology Ltd., 300 order copper powders), magnetic agitation forms suspension; After Keep agitation 30 min, by suspension centrifugal analysis, namely solid vacuum-drying is obtained hydrophobic copper powder to constant weight.
It is the α ω – dialkyl polydimethylsiloxane of 10000 cp by 5 g viscosity, 0.25 g solidifying agent tetraethoxysilane and 0.02 g catalyst dibutyltin cinnamic acid di-n-butyl tin are at room temperature dissolved in 20 mL normal hexanes, obtain room temperature vulcanized silicone rubber precursor solution.Then precursor solution is poured over surface of plate glass, and is launched into the shape of 10 cm × 10 cm with glass stick, at room temperature vacuum defoamation 5 min after natural levelling.The hydrophobic copper powder of 20 g is put into 200 order stainless steel sub-sieves, it is evenly sieved and drops on room temperature vulcanized silicone rubber precursor solution surface, after at room temperature solidifying 24 h subsequently.Finally repeatedly scrub sample surfaces with test-tube brush and tap water, after removing the hydrophobic copper powder adhered to loosely, namely obtain the room temperature vulcanized silicone rubber super hydrophobic surface of hydrophobic copper powder modification.Optical contact angle tester detects, and the static contact angle of 5 μ L deionized waters on this surface is 155.3 °.
Embodiment 6
It is the α ω – dialkyl polydimethylsiloxane of 1000 cp by 10 g viscosity, 0.5 g solidifying agent tetraethoxysilane and 0.03 g catalyst dibutyltin cinnamic acid di-n-butyl tin are at room temperature dissolved in 5 mL normal hexanes, obtain room temperature vulcanized silicone rubber precursor solution.Then precursor solution is poured over surface of plate glass, and is launched into the shape of 10 cm × 10 cm with glass stick, at room temperature vacuum defoamation 5 min after natural levelling.Be that the polytetrafluorethylepowder powder (Du Pont, ptfe micropowder, MP1200) of 3 μm puts into 200 order stainless steel sub-sieves by 20 g particle diameters, by its evenly sieve drop on room temperature vulcanized silicone rubber precursor solution surface, after at room temperature solidifying 24 h subsequently.Finally repeatedly scrub sample surfaces with test-tube brush and tap water, after removing the polytetrafluorethylepowder powder adhered to loosely, namely obtain polytetrafluoroethylmodified modified room temperature vulcanized silicone rubber super hydrophobic surface.Optical contact angle tester detects, and the static contact angle of 5 μ L deionized waters on this surface is 157.2 °.
Claims (5)
1. a preparation method for room temperature vulcanized silicone rubber super hydrophobic surface, is characterized in that preparation process comprises three steps:
The first step, by 100 weight part α ω – dialkyl polydimethylsiloxanes, 4 ~ 6 weight part solidifying agent tetraethoxysilanes, the solvent hexane of 0.1 ~ 0.5 part by weight of catalyst di-n-butyltin dilaurate and 20 ~ 100 weight parts is configured to viscous solution, the solution film of 200 ~ 2000 μm of thickness is become in sheet glass top casting, and at room temperature vacuum defoamation;
Second step, is evenly sieved the drainage powder additive of 5 ~ 20 weight parts by 80 ~ 400 order stainless steel sub-sieves and drops on above-mentioned uncured room temperature vulcanized silicone rubber viscous solution film surface, and make it cover whole surface completely;
3rd step, room temperature leaves standstill after 24 hours and namely the removing of surface residual powder is obtained room temperature vulcanized silicone rubber super hydrophobic surface.
2. the preparation method of a kind of room temperature vulcanized silicone rubber super hydrophobic surface as claimed in claim 1, is characterized in that: the viscosity of described α ， ω – dialkyl polydimethylsiloxane is 1000 ~ 20000 cp.
3. the preparation method of a kind of room temperature vulcanized silicone rubber super hydrophobic surface as claimed in claim 1, is characterized in that: described drainage powder is the one in dodecyl triethoxyl silane modification infusorial earth powder, Octadecane base trichlorosilane improved silica powder, the modified oxidized zinc powder of n-dodecyl mereaptan, Octadecane base Trimethoxy silane modified titanium dioxide powder, n-dodecyl mereaptan modification copper powder, dodecyl triethoxyl silane modified aluminium powder and polytetrafluoroethylene powder.
4. the preparation method of a kind of room temperature vulcanized silicone rubber super hydrophobic surface as claimed in claim 1, is characterized in that: described drainage powder particle diameter is 10 nm ~ 20 μm.
5. the preparation method of a kind of room temperature vulcanized silicone rubber super hydrophobic surface as claimed in claim 1, is characterized in that: described surface residual powder is removed and used tap water and test-tube brush repeatedly to wash away to constant weight.
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Cited By (14)
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| CN104761743A (en) * | 2015-04-24 | 2015-07-08 | 南昌航空大学 | Simple general preparation method of silicone rubber super-hydrophobic surface |
| CN104804208A (en) * | 2015-05-13 | 2015-07-29 | 南昌航空大学 | Preparation method for anti-icing silicone rubber composite material surface |
| CN105694715A (en) * | 2016-03-28 | 2016-06-22 | 南昌航空大学 | Preparation method of SiO2/PDMS composite transparent super hydrophobic coating |
| CN110204902A (en) * | 2019-05-31 | 2019-09-06 | 华南理工大学 | A kind of flexible bendable, active deicing super-hydrophobic ice-covering-proof composite material and preparation method and application |
| CN110330925A (en) * | 2019-06-04 | 2019-10-15 | 中电鼎康（天长）科技有限公司 | A kind of sensor potent moisture-proof adhesive and preparation method thereof |
| CN110862542A (en) * | 2019-11-29 | 2020-03-06 | 江西省科学院应用化学研究所 | Preparation method of functionalized alkoxy-containing polysiloxane |
| CN112608678A (en) * | 2021-01-12 | 2021-04-06 | 黑龙江大学 | Preparation method and application of super-hydrophobic antifouling water-saving coating |
| CN113354347A (en) * | 2021-07-15 | 2021-09-07 | 贵州大学 | Composite waterproof agent for building 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 |
| CN116410629A (en) * | 2022-01-05 | 2023-07-11 | 中国科学院青海盐湖研究所 | Super-hydrophobic powder material and preparation method and application thereof |
| WO2023130822A1 (en) * | 2022-01-08 | 2023-07-13 | 海南摩尔兄弟科技有限公司 | Hydrophobic silicone rubber, preparation method therefor, atomizer, and electronic atomization device |
| CN116426215A (en) * | 2023-04-28 | 2023-07-14 | 中国南方电网有限责任公司超高压输电公司大理局 | Composite coating, preparation method thereof, silicone rubber protective sleeve and insulator |
| CN116694228A (en) * | 2023-05-17 | 2023-09-05 | 国网山东省电力公司微山县供电公司 | Anti-aging anti-pollution flashover coating and application method thereof |
| CN116987389A (en) * | 2023-09-27 | 2023-11-03 | 唐山三孚纳米材料有限公司 | High-transparency silicon rubber composite material and preparation method thereof |
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| CN104761743A (en) * | 2015-04-24 | 2015-07-08 | 南昌航空大学 | Simple general preparation method of silicone rubber super-hydrophobic surface |
| CN104804208A (en) * | 2015-05-13 | 2015-07-29 | 南昌航空大学 | Preparation method for anti-icing silicone rubber composite material surface |
| CN104804208B (en) * | 2015-05-13 | 2018-06-01 | 南昌航空大学 | A kind of preparation method on anti-freeze silicon rubber composite material surface |
| CN105694715A (en) * | 2016-03-28 | 2016-06-22 | 南昌航空大学 | Preparation method of SiO2/PDMS composite transparent super hydrophobic coating |
| CN110204902A (en) * | 2019-05-31 | 2019-09-06 | 华南理工大学 | A kind of flexible bendable, active deicing super-hydrophobic ice-covering-proof composite material and preparation method and application |
| CN110330925A (en) * | 2019-06-04 | 2019-10-15 | 中电鼎康（天长）科技有限公司 | A kind of sensor potent moisture-proof adhesive and preparation method thereof |
| CN110862542A (en) * | 2019-11-29 | 2020-03-06 | 江西省科学院应用化学研究所 | Preparation method of functionalized alkoxy-containing polysiloxane |
| CN112608678A (en) * | 2021-01-12 | 2021-04-06 | 黑龙江大学 | Preparation method and application of super-hydrophobic antifouling water-saving coating |
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| WO2023130822A1 (en) * | 2022-01-08 | 2023-07-13 | 海南摩尔兄弟科技有限公司 | Hydrophobic silicone rubber, preparation method therefor, atomizer, and electronic atomization device |
| 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 |
| CN116426215A (en) * | 2023-04-28 | 2023-07-14 | 中国南方电网有限责任公司超高压输电公司大理局 | Composite coating, preparation method thereof, silicone rubber protective sleeve and insulator |
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| CN116987389A (en) * | 2023-09-27 | 2023-11-03 | 唐山三孚纳米材料有限公司 | High-transparency silicon rubber composite material and preparation method thereof |
| CN116987389B (en) * | 2023-09-27 | 2024-01-12 | 唐山三孚纳米材料有限公司 | High-transparency silicon rubber composite material and preparation method thereof |
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