CN108912985A - A kind of hydrophobic coating and preparation method thereof - Google Patents
A kind of hydrophobic coating and preparation method thereof Download PDFInfo
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- CN108912985A CN108912985A CN201710166212.0A CN201710166212A CN108912985A CN 108912985 A CN108912985 A CN 108912985A CN 201710166212 A CN201710166212 A CN 201710166212A CN 108912985 A CN108912985 A CN 108912985A
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- 238000000576 coating method Methods 0.000 title claims abstract description 45
- 239000011248 coating agent Substances 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- 230000002209 hydrophobic effect Effects 0.000 title claims description 17
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims abstract description 57
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims abstract description 38
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 36
- 238000003756 stirring Methods 0.000 claims abstract description 24
- ABTOQLMXBSRXSM-UHFFFAOYSA-N silicon tetrafluoride Chemical compound F[Si](F)(F)F ABTOQLMXBSRXSM-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000002270 dispersing agent Substances 0.000 claims abstract description 20
- 239000011347 resin Substances 0.000 claims abstract description 20
- 229920005989 resin Polymers 0.000 claims abstract description 20
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 19
- 239000002245 particle Substances 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- QQQSFSZALRVCSZ-UHFFFAOYSA-N triethoxysilane Chemical compound CCO[SiH](OCC)OCC QQQSFSZALRVCSZ-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000002253 acid Substances 0.000 claims abstract description 11
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 51
- 238000000034 method Methods 0.000 claims description 40
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 21
- -1 perfluoro Chemical group 0.000 claims description 16
- 239000004814 polyurethane Substances 0.000 claims description 9
- 229920002635 polyurethane Polymers 0.000 claims description 9
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 8
- 229910052710 silicon Inorganic materials 0.000 claims description 8
- 239000010703 silicon Substances 0.000 claims description 8
- 239000005056 polyisocyanate Substances 0.000 claims description 4
- 229920001228 polyisocyanate Polymers 0.000 claims description 4
- 239000004925 Acrylic resin Substances 0.000 claims description 3
- 229920000178 Acrylic resin Polymers 0.000 claims description 3
- 239000003973 paint Substances 0.000 claims description 2
- 239000004034 viscosity adjusting agent Substances 0.000 claims description 2
- 239000000243 solution Substances 0.000 claims 7
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims 2
- YESRULSVSWLZLT-UHFFFAOYSA-N C(C)O[SiH](OCC)OCC.[Ru].[F] Chemical compound C(C)O[SiH](OCC)OCC.[Ru].[F] YESRULSVSWLZLT-UHFFFAOYSA-N 0.000 claims 1
- 150000002148 esters Chemical class 0.000 claims 1
- 239000011259 mixed solution Substances 0.000 claims 1
- 230000003075 superhydrophobic effect Effects 0.000 abstract description 34
- 239000000126 substance Substances 0.000 abstract description 5
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 24
- 239000000758 substrate Substances 0.000 description 8
- QTRSWYWKHYAKEO-UHFFFAOYSA-N 1,1,2,2,3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10-henicosafluorodecyl-tris(1,1,2,2,2-pentafluoroethoxy)silane Chemical compound FC(F)(F)C(F)(F)O[Si](OC(F)(F)C(F)(F)F)(OC(F)(F)C(F)(F)F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F QTRSWYWKHYAKEO-UHFFFAOYSA-N 0.000 description 6
- 238000009740 moulding (composite fabrication) Methods 0.000 description 5
- 230000005540 biological transmission Effects 0.000 description 3
- 230000007423 decrease Effects 0.000 description 3
- 239000002105 nanoparticle Substances 0.000 description 3
- 238000001035 drying Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229920001971 elastomer Polymers 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 230000006641 stabilisation Effects 0.000 description 2
- 238000011105 stabilization Methods 0.000 description 2
- HBGPNLPABVUVKZ-POTXQNELSA-N (1r,3as,4s,5ar,5br,7r,7ar,11ar,11br,13as,13br)-4,7-dihydroxy-3a,5a,5b,8,8,11a-hexamethyl-1-prop-1-en-2-yl-2,3,4,5,6,7,7a,10,11,11b,12,13,13a,13b-tetradecahydro-1h-cyclopenta[a]chrysen-9-one Chemical compound C([C@@]12C)CC(=O)C(C)(C)[C@@H]1[C@H](O)C[C@]([C@]1(C)C[C@@H]3O)(C)[C@@H]2CC[C@H]1[C@@H]1[C@]3(C)CC[C@H]1C(=C)C HBGPNLPABVUVKZ-POTXQNELSA-N 0.000 description 1
- PFRGGOIBYLYVKM-UHFFFAOYSA-N 15alpha-hydroxylup-20(29)-en-3-one Natural products CC(=C)C1CCC2(C)CC(O)C3(C)C(CCC4C5(C)CCC(=O)C(C)(C)C5CCC34C)C12 PFRGGOIBYLYVKM-UHFFFAOYSA-N 0.000 description 1
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 description 1
- SOKRNBGSNZXYIO-UHFFFAOYSA-N Resinone Natural products CC(=C)C1CCC2(C)C(O)CC3(C)C(CCC4C5(C)CCC(=O)C(C)(C)C5CCC34C)C12 SOKRNBGSNZXYIO-UHFFFAOYSA-N 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 238000004378 air conditioning Methods 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- ZHPNWZCWUUJAJC-UHFFFAOYSA-N fluorosilicon Chemical compound [Si]F ZHPNWZCWUUJAJC-UHFFFAOYSA-N 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000005057 refrigeration Methods 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- 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
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/04—Polyurethanes
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- 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
- C09D133/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Paints Or Removers (AREA)
- Application Of Or Painting With Fluid Materials (AREA)
Abstract
The present invention provides the super hydrophobic coatings and preparation method thereof that a kind of water contact angle is greater than 150 °, include the following steps：Perfluoro capryl triethoxysilane is added into ethanol solution, with second acid for adjusting pH value less than 7, stirring；TiO is added2, it stirs, is centrifugated, it is dry, the TiO of silicon fluoride hydrophobically modified is made2Particle；The TiO of silicon fluoride hydrophobically modified is added into dimethylbenzene and ethyl acetate solution2Particle, dispersing agent, modified resin and curing agent；Stirring adjusts viscosity, and super hydrophobic coating is made.The super hydrophobic coating performance is stablized, and the introducing of inorganic particulate improves the wearability of coating, while the introducing of low-surface energy substance silicon fluoride, further reduced the surface tension of coating.
Description
Technical field
The present invention relates to paint fields, more particularly, to a kind of hydrophobic coating and preparation method thereof.
Background technique
It freezes, frost is widely present in refrigeration system (the anti-frost of such as air-conditioning), transmission line of electricity, fan blade table
Face, building exterior wall surface, aircraft surfaces (such as surface of wing, air intake duct, windshield).The presence of ice (frost) layer makes equipment
The coefficient of overall heat transmission reduces, and crushing increases, and generates large effect to system；Fan blade surface then needs to bear various high wind sand, rain
The erosion of the natural causes such as water, frost, ultraviolet radiation and the abrasion to run at high speed；Transmission line of electricity, flies at building exterior wall surface
The anti-icing performance on machine surface etc. is also most important.
The film forming matter that existing hydrophobic product uses is that low-surface energy substance is constituted, and mostly contains fluorine, so that the knot at interface
It is poor with joint efforts, cannot be used for a long time, and in multiple icing-ice-melt circulation, hydrophobic performance decline is obvious, some coatings it is resistance to
Mill property is poor, and particle easily falls off from surface and loses hydrophobic effect.
Therefore, it is badly in need of studying the coating that a kind of hydrophobic performance is stable and wearability is good.
Summary of the invention
To solve the above-mentioned problems, the present invention is using silicon fluoride to the TiO of micron and nanometer particle size2Particle carries out surface and changes
Property, and using the hydrolysis of acetic acid promotion silicon fluoride, so that the surface of nanoparticle is assigned its surface super-hydrophobic with hydrophobic grouping
Matter, keeps the stabilization of ultra-hydrophobicity, while selecting the preferable modified resin of film forming, improves the wearability of coating, and
Low-surface energy substance is introduced when nanometer particle-modified, further decreases the surface tension of coating.
The present invention provides a kind of methods for preparing hydrophobic coating, include the following steps：Fluorine silicon is added into ethanol solution
Alkane, with second acid for adjusting pH, stirring；TiO is added2, it stirs, is centrifugated, it is dry, the TiO of silicon fluoride hydrophobically modified is made2Particle；
The TiO of the silicon fluoride hydrophobically modified is added into dimethylbenzene and ethyl acetate solution2Particle, dispersing agent, modified resin and solid
Agent；And stirring, viscosity is adjusted, hydrophobic coating is made.
In the above-mentioned methods, hydrophobic coating is the super hydrophobic coating that water contact angle is greater than 150 °.
In the above-mentioned methods, silicon fluoride, TiO2, dispersing agent, modified resin and curing agent mass ratio be 2~8：4~12：
6~40：7~60：9.
In the above-mentioned methods, silicon fluoride is perfluoro capryl triethoxysilane or perfluoro decyl triethoxysilane.
In the above-mentioned methods, perfluoro capryl triethoxysilane or perfluoro decyl triethoxysilane are in ethanol solution
Mass fraction is 1~3%.
In the above-mentioned methods, perfluoro capryl triethoxysilane or perfluoro decyl triethoxysilane are in ethanol solution
Mass fraction is 2%.
In the above-mentioned methods, the acetic acid for being 36%~38% with mass fraction adjusts solution ph less than 7.
In the above-mentioned methods, TiO2For the TiO of 10~30nm partial size2With the TiO of 150~250nm partial size2Different-grain diameter
TiO2；It is preferred that the TiO of 20nm partial size2With the TiO of 200nm partial size2。
In the above-mentioned methods, the TiO of 10~30nm partial size2With the TiO of 150~250nm partial size2Mass ratio be 1:1.
In the above-mentioned methods, the volume ratio of the dimethylbenzene and ethyl acetate of dimethylbenzene and ethyl acetate solution is 1:1.
In the above-mentioned methods, the volume ratio of ethanol solution and dimethylbenzene and ethyl acetate solution is 1:0.7~0.8.
In the above-mentioned methods, dispersing agent is BYK dispersing agent, and BYK dispersing agent includes BYK-161, BYK-163 and BYK-110
It is one or more.
In the above-mentioned methods, modified resin be organic silicon modified polyurethane and organosilicon modified crylic acid resin one kind or
Two kinds.
In the above-mentioned methods, curing agent is polyisocyanates, and polyisocyanates includes N75 curing agent (Bayer Bitterfeld GmbH).
In the above-mentioned methods, viscosity-adjusting agent is 15~20Pas.
The present invention also provides a kind of hydrophobic coatings prepared according to above method.
The super hydrophobic coating of the method preparation provided through the invention has hydrophobic automatically cleaning and ice-covering-proof effect, and
Ultra-hydrophobicity is stablized, and the film formings such as organic silicon modified polyurethane and/or organosilicon modified crylic acid resin is selected preferably to change
Property resin, improve the wearability of coating, at the same when nanometer particle-modified introduce low-surface energy substance silicon fluoride, further drop
The low surface tension of coating.Efficiently solve the problems, such as that ultra-hydrophobicity is unstable and wearability is poor.
Detailed description of the invention
Fig. 1 is the preparation flow figure of super hydrophobic coating.
Specific embodiment
The following examples can make those skilled in the art that the present invention be more fully understood, but not limit in any way
The present invention.
TiO of the present invention to micron and nanometer particle size2Particle carries out surface and is modified, and assigns its surface super hydrophobic property, protects
The stabilization of ultra-hydrophobicity has been demonstrate,proved, and has selected the preferable modified resin of film forming, has improved the wearability of coating, low-surface-energy object
The introducing of matter further decreases the surface tension of coating.
The present invention provides a kind of methods for preparing super hydrophobic coating of the water contact angle greater than 150 °, include the following steps：
Perfluoro capryl triethoxysilane or three second of perfluoro decyl is added in ethanol solution (analysis that mass fraction is 99.7% is pure)
Oxysilane, wherein the quality of perfluoro capryl triethoxysilane or perfluoro decyl triethoxysilane in ethanol solution point
Number is 2%；With mass fraction be 36%~38% second acid for adjusting pH value less than 7, stirring 20~for 24 hours；
TiO is added2, 4~6h of stirring, 30~50min of centrifuge separation, drying 20~for 24 hours, silicon fluoride hydrophobically modified is made
TiO2Particle is denoted as FAS-TiO2；Wherein, TiO2For the TiO of 10~30nm partial size2With the TiO of 150~250nm partial size2Difference
The TiO of partial size2, the preferably TiO of 20nm partial size2With the TiO of 200nm partial size2；The TiO of 10~30nm partial size2With 150~250nm
The TiO of partial size2Mass ratio be 1:1；
FAS-TiO is added into dimethylbenzene and ethyl acetate solution2, BYK dispersing agent, modified resin and curing agent；And
30~60min is stirred, adjusting viscosity is 15~20Pas, and super hydrophobic coating is made；Wherein, dimethylbenzene and ethyl acetate solution
Dimethylbenzene and ethyl acetate volume ratio be 1:1；The volume ratio of ethanol solution and dimethylbenzene and ethyl acetate solution is 1:0.7
~0.8；BYK dispersing agent includes the one or more of BYK-161, BYK-163 and BYK-110；Modified resin is organic-silicon-modified
The one or two of polyurethane and organosilicon modified crylic acid resin；Curing agent is polyisocyanates, including N75 curing agent；
Wherein, perfluoro capryl triethoxysilane, TiO2, dispersing agent, modified resin and curing agent mass ratio be 2~8：
4~12：6~40：7~60：9.
The super hydrophobic coating is sprayed or brushed to substrate surface to get super hydrophobic surface.
Embodiment one
2g perfluoro capryl triethoxysilane is added into 98g ethanol solution, is adjusted with the acetic acid that mass fraction is 36%
PH value is less than 7, and stirring is for 24 hours；
The TiO of 20nm partial size is added2With the TiO of 200nm partial size2Total 10g stirs 4h, is centrifugated 50min, dries for 24 hours,
The TiO of silicon fluoride hydrophobically modified is made2Particle is denoted as FAS-TiO2；
FAS-TiO is added into 50mL dimethylbenzene and 50mL ethyl acetate mixture2, 6g dispersant B YK-110,50g
Organic silicon modified polyurethane and 9g N75 curing agent；
30min is stirred, adjusting viscosity is 15Pas, and super hydrophobic coating is made；
The super hydrophobic coating is sprayed or brushed to substrate surface to get super hydrophobic surface, water contact angle, wearability are tested
And surface tension.
Embodiment two
6g perfluoro decyl triethoxysilane is added into 194g ethanol solution, is adjusted with the acetic acid that mass fraction is 38%
PH value stirs 20h less than 7；
The TiO of 15nm partial size is added2With the TiO of 250nm partial size2Total 12g stirs 6h, is centrifugated 40min, dry 22h,
The TiO of silicon fluoride hydrophobically modified is made2Particle is denoted as FAS-TiO2；
FAS-TiO is added into 85mL dimethylbenzene and 85mL ethyl acetate mixture2, 30g dispersant B YK-161,40g
Organic silicon modified polyurethane and 9g N75 curing agent；
50min is stirred, adjusting viscosity is 20Pas, and super hydrophobic coating is made；
The super hydrophobic coating is sprayed or brushed to substrate surface to get super hydrophobic surface, water contact angle, wearability are tested
And surface tension.
Embodiment three
8g perfluoro capryl triethoxysilane is added into 392g ethanol solution, is adjusted with the acetic acid that mass fraction is 37%
PH value stirs 23h less than 7；
The TiO of 30nm partial size is added2With the TiO of 150nm partial size2Total 12g stirs 5h, is centrifugated 30min, dry 20h,
The TiO of silicon fluoride hydrophobically modified is made2Particle is denoted as FAS-TiO2；
FAS-TiO is added into 180mL dimethylbenzene and 180mL ethyl acetate solution2, 40g dispersant B YK-163,60g have
Machine fluorine-silicon modified acrylic resin and 9g N75 curing agent；
60min is stirred, adjusting viscosity is 18Pas, and super hydrophobic coating is made；
The super hydrophobic coating is sprayed or brushed to substrate surface to get super hydrophobic surface, water contact angle, wearability are tested
And surface tension.
Example IV
2g perfluoro capryl triethoxysilane is added into 198g ethanol solution, is adjusted with the acetic acid that mass fraction is 37%
PH value stirs 20h less than 7；
The TiO of 10nm partial size is added2With the TiO of 225nm partial size2Total 4g stirs 6h, is centrifugated 40min, dry 21h,
The TiO of silicon fluoride hydrophobically modified is made2Particle is denoted as FAS-TiO2；
FAS-TiO is added into 100mL dimethylbenzene and 100mL ethyl acetate solution2, 7g dispersant B YK-110,7g it is organic
Fluorine-silicon modified acrylic resin and 9g N75 curing agent；
30min is stirred, adjusting viscosity is 20Pas, and super hydrophobic coating is made；
The super hydrophobic coating is sprayed or brushed to substrate surface to get super hydrophobic surface, water contact angle, wearability are tested
And surface tension.
Embodiment five
2g perfluoro decyl triethoxysilane is added into 98g ethanol solution, is adjusted with the acetic acid that mass fraction is 36%
PH value stirs 22h less than 7；
The TiO of 20nm partial size is added2With the TiO of 200nm partial size2Total 9g stirs 6h, is centrifugated 40min, dry 21h,
The TiO of silicon fluoride hydrophobically modified is made2Particle is denoted as FAS-TiO2；
FAS-TiO is added into 50mL dimethylbenzene and 50mL ethyl acetate solution2, 20g dispersant B YK-110,60g it is organic
Silicon modified polyurethane and organosilicon modified crylic acid resin and 9g N75 curing agent；
60min is stirred, adjusting viscosity is 15Pas, and super hydrophobic coating is made；
The super hydrophobic coating is sprayed or brushed to substrate surface to get super hydrophobic surface, water contact angle, wearability are tested
And surface tension.
Embodiment six
2g perfluoro capryl triethoxysilane is added into 98g ethanol solution, is adjusted with the acetic acid that mass fraction is 38%
PH value is less than 7, and stirring is for 24 hours；
The TiO of 20nm partial size is added2With the TiO of 200nm partial size2Total 10g stirs 5h, is centrifugated 50min, dry 23h,
The TiO of silicon fluoride hydrophobically modified is made2Particle is denoted as FAS-TiO2；
FAS-TiO is added into 50mL dimethylbenzene and 50mL ethyl acetate solution2, 6g dispersant B YK-110,50g it is organic
Silicon modified polyurethane and organosilicon modified crylic acid resin and 9g N75 curing agent；
60min is stirred, adjusting viscosity is 18Pas, and super hydrophobic coating is made；
The super hydrophobic coating is sprayed or brushed to substrate surface to get super hydrophobic surface, water contact angle, wearability are tested
And surface tension.
The above stirring is all made of the revolving speed of 3000~4000r/min, and centrifuge separation is turned using 4000~6000r/min's
Speed, drying temperature are 80 DEG C.
The test method of the above water contact angle is sessile drop method commonly used in the art, and 5 μ L of test droplets, test equipment is
OCA20- contact angle tester；Wearability then use GB/T1768-2006 commonly used in the art (rotation rubber grinding wheel method) and
GB/T 23988-2009 (knockout method) measurement；Surface tension is measured using Sigma 702ET surface and interface tensiometer；Senile experiment
It is measured using GB/T 14522-2008 standard, and using Q8/UV ultraviolet light accelerated weathering accelerator.
Water contact angle, wearability and the surface tension result that embodiment one to six is tested are as follows：
Table 1, test result
Seen from table 1, the water contact angle of the super hydrophobic coating provided using nano particle surface modifying is greater than 150 °, reaches
Good super-hydrophobic effect, and it is steady by the ultra-hydrophobicity that Q8/UV senile experiment can be seen that the super hydrophobic coating
It is fixed；The use of modified resin organic silicon modified polyurethane and organosilicon modified crylic acid resin increases the resistance to of super hydrophobic coating
Mill property, whether GB/T 1768-2006 (rotation rubber grinding wheel method) or GB/T 23988-2009 (knockout method) measurement, all far
It has been more than standard, and the good film-forming property of modified resin, can have been combined well with substrate surface；Nanoparticle surface changes simultaneously
Property introduce low-surface energy substance silicon fluoride, further reduced the surface tension of system.
It will be understood by those skilled in the art that above embodiments are only exemplary embodiments, without departing substantially from spirit of the invention
In the case where range, a variety of variations can be carried out, replaced and changed.
Claims (16)
1. a kind of method for preparing hydrophobic coating, which is characterized in that include the following steps：
Silicon fluoride is added into ethanol solution, with second acid for adjusting pH, stirring；
TiO is added2, it stirs, is centrifugated, it is dry, the TiO of silicon fluoride hydrophobically modified is made2Particle；
The TiO of the silicon fluoride hydrophobically modified is added into dimethylbenzene and ethyl acetate solution2Particle, dispersing agent, modified resin and
Curing agent；And
Stirring adjusts viscosity, the hydrophobic coating is made.
2. the method according to claim 1, wherein the hydrophobic coating is that water contact angle is super thin greater than 150 °
Water paint.
3. the method according to claim 1, wherein the silicon fluoride, the TiO2, the dispersing agent, described change
Property resin and the curing agent mass ratio be 2~8：4~12：6~40：7~60：9.
4. the method according to claim 1, wherein the silicon fluoride is for perfluoro capryl triethoxysilane or entirely
Fluorine ruthenium triethoxysilane.
5. according to the method described in claim 4, it is characterized in that, the perfluoro capryl triethoxysilane or the perfluor last of the ten Heavenly stems
Mass fraction of the ethyl triethoxy silicane alkane in the ethanol solution is 1~3%.
6. according to the method described in claim 5, it is characterized in that, the perfluoro capryl triethoxysilane or the perfluor last of the ten Heavenly stems
Mass fraction of the ethyl triethoxy silicane alkane in the ethanol solution is 2%.
7. the method according to claim 1, wherein the second acid-conditioning solution for being 36%~38% with mass fraction
PH value is less than 7.
8. the method according to claim 1, wherein the TiO2For the TiO of 10~30nm partial size2With 150~
The TiO of 250nm partial size2Different-grain diameter TiO2。
9. according to the method described in claim 8, it is characterized in that, the TiO of 10~30nm partial size2With described 150~
The TiO of 250nm partial size2Mass ratio be 1:1.
10. the method according to claim 1, wherein the dimethylbenzene of the dimethylbenzene and ethyl acetate solution and
The volume ratio of ethyl acetate is 1:1.
11. the method according to claim 1, wherein the ethanol solution and the dimethylbenzene and ethyl acetate
The volume ratio of mixed solution is 1:0.7~0.8.
12. the method according to claim 1, wherein the dispersing agent is BYK dispersing agent, the BYK dispersing agent
Including the one or more of BYK-161, BYK-163 and BYK-110.
13. the method according to claim 1, wherein the modified resin is organic silicon modified polyurethane and has
The one or two of machine fluorine-silicon modified acrylic resin.
14. the method according to claim 1, wherein the curing agent is polyisocyanates, the polyisocyanic acid
Ester includes N75 curing agent.
15. the method according to claim 1, wherein the viscosity-adjusting agent is 15~20Pas.
16. a kind of hydrophobic coating of the preparation of method described in any one of -15 according to claim 1.
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