CN112175520A - Preparation method and application of super-hydrophobic, transparent and durable coating - Google Patents
Preparation method and application of super-hydrophobic, transparent and durable coating Download PDFInfo
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- CN112175520A CN112175520A CN202010854161.2A CN202010854161A CN112175520A CN 112175520 A CN112175520 A CN 112175520A CN 202010854161 A CN202010854161 A CN 202010854161A CN 112175520 A CN112175520 A CN 112175520A
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- silane
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- 239000011248 coating agent Substances 0.000 title claims abstract description 66
- 238000000576 coating method Methods 0.000 title claims abstract description 66
- 230000003075 superhydrophobic effect Effects 0.000 title claims abstract description 49
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 239000002105 nanoparticle Substances 0.000 claims abstract description 38
- 239000011347 resin Substances 0.000 claims abstract description 32
- 229920005989 resin Polymers 0.000 claims abstract description 32
- 238000005507 spraying Methods 0.000 claims abstract description 19
- 238000004528 spin coating Methods 0.000 claims abstract description 18
- 239000007788 liquid Substances 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 10
- 239000000463 material Substances 0.000 claims abstract description 7
- 239000011159 matrix material Substances 0.000 claims abstract description 4
- VBGGLSWSRVDWHB-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(trifluoromethoxy)silane Chemical compound FC(F)(F)O[Si](OC(F)(F)F)(OC(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 VBGGLSWSRVDWHB-UHFFFAOYSA-N 0.000 claims description 22
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 22
- 239000000725 suspension Substances 0.000 claims description 22
- 239000000758 substrate Substances 0.000 claims description 21
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 18
- 229910000077 silane Inorganic materials 0.000 claims description 18
- 239000000243 solution Substances 0.000 claims description 18
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 15
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 claims description 14
- 239000012975 dibutyltin dilaurate Substances 0.000 claims description 14
- PHQOGHDTIVQXHL-UHFFFAOYSA-N n'-(3-trimethoxysilylpropyl)ethane-1,2-diamine Chemical compound CO[Si](OC)(OC)CCCNCCN PHQOGHDTIVQXHL-UHFFFAOYSA-N 0.000 claims description 14
- 238000009210 therapy by ultrasound Methods 0.000 claims description 14
- 239000000377 silicon dioxide Substances 0.000 claims description 13
- HQYALQRYBUJWDH-UHFFFAOYSA-N trimethoxy(propyl)silane Chemical compound CCC[Si](OC)(OC)OC HQYALQRYBUJWDH-UHFFFAOYSA-N 0.000 claims description 13
- 239000003795 chemical substances by application Substances 0.000 claims description 12
- 239000011259 mixed solution Substances 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 11
- 239000002904 solvent Substances 0.000 claims description 11
- 238000003756 stirring Methods 0.000 claims description 10
- 239000007921 spray Substances 0.000 claims description 8
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 6
- 125000003700 epoxy group Chemical group 0.000 claims description 6
- 239000011521 glass Substances 0.000 claims description 5
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 4
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 4
- OBNDGIHQAIXEAO-UHFFFAOYSA-N [O].[Si] Chemical group [O].[Si] OBNDGIHQAIXEAO-UHFFFAOYSA-N 0.000 claims description 4
- 239000003607 modifier Substances 0.000 claims description 4
- -1 polydimethylsiloxane Polymers 0.000 claims description 4
- 230000004048 modification Effects 0.000 claims description 3
- 238000012986 modification Methods 0.000 claims description 3
- KKYDYRWEUFJLER-UHFFFAOYSA-N 1,1,2,2,3,3,4,4,5,5,6,6,7,7,10,10,10-heptadecafluorodecyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)CCC(F)(F)F KKYDYRWEUFJLER-UHFFFAOYSA-N 0.000 claims description 2
- ZWVDTRNPSDMWTB-UHFFFAOYSA-N 2-methylpropylsilane Chemical compound CC(C)C[SiH3] ZWVDTRNPSDMWTB-UHFFFAOYSA-N 0.000 claims description 2
- DTOOTUYZFDDTBD-UHFFFAOYSA-N 3-chloropropylsilane Chemical compound [SiH3]CCCCl DTOOTUYZFDDTBD-UHFFFAOYSA-N 0.000 claims description 2
- IMDPTYFNMLYSLH-UHFFFAOYSA-N 3-silylpropyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OCCC[SiH3] IMDPTYFNMLYSLH-UHFFFAOYSA-N 0.000 claims description 2
- AFUWHLXUBJOPNO-UHFFFAOYSA-N CCCCCCCCCCCCCCCC[SiH3] Chemical compound CCCCCCCCCCCCCCCC[SiH3] AFUWHLXUBJOPNO-UHFFFAOYSA-N 0.000 claims description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 2
- 230000032683 aging Effects 0.000 claims description 2
- 125000003277 amino group Chemical group 0.000 claims description 2
- 239000003054 catalyst Substances 0.000 claims description 2
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 2
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 claims description 2
- RSKGMYDENCAJEN-UHFFFAOYSA-N hexadecyl(trimethoxy)silane Chemical compound CCCCCCCCCCCCCCCC[Si](OC)(OC)OC RSKGMYDENCAJEN-UHFFFAOYSA-N 0.000 claims description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 2
- UIUXUFNYAYAMOE-UHFFFAOYSA-N methylsilane Chemical compound [SiH3]C UIUXUFNYAYAMOE-UHFFFAOYSA-N 0.000 claims description 2
- YTJSFYQNRXLOIC-UHFFFAOYSA-N octadecylsilane Chemical compound CCCCCCCCCCCCCCCCCC[SiH3] YTJSFYQNRXLOIC-UHFFFAOYSA-N 0.000 claims description 2
- SLYCYWCVSGPDFR-UHFFFAOYSA-N octadecyltrimethoxysilane Chemical compound CCCCCCCCCCCCCCCCCC[Si](OC)(OC)OC SLYCYWCVSGPDFR-UHFFFAOYSA-N 0.000 claims description 2
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 2
- PARWUHTVGZSQPD-UHFFFAOYSA-N phenylsilane Chemical compound [SiH3]C1=CC=CC=C1 PARWUHTVGZSQPD-UHFFFAOYSA-N 0.000 claims description 2
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 2
- 229920000642 polymer Polymers 0.000 claims description 2
- UIDUKLCLJMXFEO-UHFFFAOYSA-N propylsilane Chemical compound CCC[SiH3] UIDUKLCLJMXFEO-UHFFFAOYSA-N 0.000 claims description 2
- 150000004756 silanes Chemical class 0.000 claims description 2
- 235000012239 silicon dioxide Nutrition 0.000 claims description 2
- TXDNPSYEJHXKMK-UHFFFAOYSA-N sulfanylsilane Chemical compound S[SiH3] TXDNPSYEJHXKMK-UHFFFAOYSA-N 0.000 claims description 2
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 2
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 claims description 2
- 239000004408 titanium dioxide Substances 0.000 claims description 2
- BPCXHCSZMTWUBW-UHFFFAOYSA-N triethoxy(1,1,2,2,3,3,4,4,5,5,8,8,8-tridecafluorooctyl)silane Chemical compound CCO[Si](OCC)(OCC)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)CCC(F)(F)F BPCXHCSZMTWUBW-UHFFFAOYSA-N 0.000 claims description 2
- 125000001153 fluoro group Chemical group F* 0.000 claims 2
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 claims 1
- 238000004140 cleaning Methods 0.000 abstract description 6
- 239000006185 dispersion Substances 0.000 abstract description 6
- 230000002209 hydrophobic effect Effects 0.000 abstract description 6
- 239000000853 adhesive Substances 0.000 abstract description 3
- 230000001070 adhesive effect Effects 0.000 abstract description 3
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 239000002131 composite material Substances 0.000 abstract description 2
- 239000000203 mixture Substances 0.000 description 32
- 229910052681 coesite Inorganic materials 0.000 description 8
- 229910052906 cristobalite Inorganic materials 0.000 description 8
- 229910052682 stishovite Inorganic materials 0.000 description 8
- 229910052905 tridymite Inorganic materials 0.000 description 8
- 239000002253 acid Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 238000012360 testing method Methods 0.000 description 3
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 239000004744 fabric Substances 0.000 description 2
- 229910052731 fluorine Inorganic materials 0.000 description 2
- 239000011737 fluorine Substances 0.000 description 2
- 239000002987 primer (paints) Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 230000003068 static effect Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000002834 transmittance Methods 0.000 description 2
- VDBJCDWTNCKRTF-UHFFFAOYSA-N 6'-hydroxyspiro[2-benzofuran-3,9'-9ah-xanthene]-1,3'-dione Chemical compound O1C(=O)C2=CC=CC=C2C21C1C=CC(=O)C=C1OC1=CC(O)=CC=C21 VDBJCDWTNCKRTF-UHFFFAOYSA-N 0.000 description 1
- 240000002853 Nelumbo nucifera Species 0.000 description 1
- 235000006508 Nelumbo nucifera Nutrition 0.000 description 1
- 235000006510 Nelumbo pentapetala Nutrition 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 229920000122 acrylonitrile butadiene styrene Polymers 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000000805 composite resin Substances 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 238000009863 impact test Methods 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
- 239000002352 surface water Substances 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 238000004078 waterproofing Methods 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
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Classifications
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- 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
- C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
- C09D183/04—Polysiloxanes
- C09D183/08—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen, and oxygen
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D5/00—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D5/00—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures
- B05D5/06—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures to obtain multicolour or other optical effects
- B05D5/061—Special surface effect
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D5/00—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures
- B05D5/08—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures to obtain an anti-friction or anti-adhesive surface
- B05D5/083—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures to obtain an anti-friction or anti-adhesive surface involving the use of fluoropolymers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
- B05D7/24—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials for applying particular liquids or other fluent materials
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/06—Preparatory processes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/22—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen and oxygen
- C08G77/26—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen and oxygen nitrogen-containing groups
-
- 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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
- C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
-
- 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
Abstract
The invention belongs to the technical field of composite hydrophobic materials, and particularly relates to a preparation method and application of a super-hydrophobic, transparent and durable coating. The modified nanoparticles are mixed with room-temperature curing resin with excellent mechanical property to obtain uniform dispersion liquid, and the dispersion liquid is deposited on the surface of a matrix in a spin coating or spraying manner to prepare the super-hydrophobic, transparent and durable coating. The prepared super-hydrophobic coating has the characteristics of simple method operation, low energy consumption, high efficiency and the like, and has excellent properties of transparency, super-hydrophobicity, good adhesive force, durability, self-cleaning and the like, so that the prepared super-hydrophobic coating has wide market application prospect.
Description
Technical Field
The invention belongs to the technical field of composite hydrophobic materials, and particularly relates to a preparation method and application of a super-hydrophobic, transparent and durable coating.
Background
The super-hydrophobic surface is a novel special surface with a static contact angle larger than 150 degrees and a rolling angle smaller than 10 degrees, is closely related to human life, has wide application value, has the characteristics of self-cleaning, antifogging, waterproofing, anti-icing, drag reduction, corrosion resistance, oil-water separation and the like, has very wide application prospect in the fields of buildings, electronics, energy, aviation and textiles, and can be used for carrying out targeted research and development on the super-hydrophobic coating according to the characteristics and requirements of different fields. After the principle of lotus leaf effect is disclosed since the teaching of Barthlott in 1997, researchers have more profound understanding on the wetting behavior of the material surface, and also further research on the construction mechanism of super-hydrophobicity and reach the consensus: firstly, the surface is constructed with certain roughness, and secondly, the surface is modified by chemical substances with low surface energy.
CN111154396A discloses a nano-silica modified silicon resin super-hydrophobic coating, a preparation method and an application thereof, wherein the nano-silica modified silicon resin super-hydrophobic coating is formed by grafting hydrophobic functional group molecules with low surface energy and high stability on the surface of nano-silica particles and then crosslinking the molecules with silicon resin, the formed nano-silica modified silicon resin super-hydrophobic coating has a super-hydrophobic surface with low surface energy and a micro-nano binary coarse structure, and the static contact angle of the super-hydrophobic coating is 159.6-161.8 degrees.
CN107868533B discloses a super-hydrophobic coating and a method for preparing a durable super-hydrophobic coating thereof, comprising: (1) primer coating: consists of 40 to 70 percent of fluororesin, 5 to 20 percent of curing agent, 0 to 10 percent of nano particles and 15 to 45 percent of solvent; (2) finishing paint: consists of fluororesin 4-30 wt%, curing agent 1-10 wt%, nanometer particle 2-10 wt% and solvent 75-85 wt%. And spraying the primer to the surfaces of different base materials, curing for a certain time at room temperature, then spraying the finish, and curing for 2-7 days at room temperature to obtain the super-hydrophobic coating film with good hardness, adhesion, flexibility, impact resistance, wear resistance, acid and alkali resistance and salt resistance. The super-hydrophobic coating material obtained by the super-hydrophobic coating has high durability and substrate universality, is suitable for large-area construction, and enables the surfaces of metal, glass, stone, wood, fabric and the like to have excellent self-cleaning, waterproof, acid and alkali resistance and corrosion resistance.
However, in the prior art, a super-hydrophobic coating with high transparency, good adhesive force, wear resistance, acid resistance, heat resistance and water resistance is not prepared efficiently and massively under the condition of low energy consumption by a simple process. The normal-temperature cured super-hydrophobic coating prepared based on the sol-gel method and the spin coating technology has more excellent mechanical stability, durability, hydrophobicity, transparency and other properties.
Disclosure of Invention
To solve some problems of the prior art, the present invention aims to provide a preparation method of a super-hydrophobic, transparent and durable coating and potential application thereof. The coating has high transparency, mechanical stability, durability and substrate universality, can be applied to the surfaces of glass, ceramics, conductive glass, aluminum, fabrics, ABS plastics and the like in a large area, and greatly improves the hydrophobicity.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a transparent super-hydrophobic coating, which comprises room temperature curing resin, a solvent and modified nanoparticles. The room temperature cured resin provides mechanical properties and partial special properties of the coating, so that the coating has certain mechanical strength, substrate bonding force, good transparency and good hydrophobicity (107 degrees). The modified nanoparticles have low surface energy grafts and high surface roughness. And combining the two to obtain uniform nano particle/resin composite super-hydrophobic coating dispersion liquid, coating the dispersion liquid on the surface of a machine body in a spin coating or spraying mode, and curing at room temperature for 24 hours to obtain the super-hydrophobic coating with excellent performance.
The super-hydrophobic, transparent and durable coating comprises room temperature curing resin, solvent and modified nano particles in the following mass ratio:
the coating comprises 14% -50% of room temperature curing resin, 50% -85% of solvent and 0.25% -3% of modified nanoparticles.
The 14-50% of room temperature curing resin comprises 0-75% of optional silane and 25-100% of essential silane;
further, 0-75% of the optional silane in the 14-50% room temperature curing resin comprises one or more of phenyl silane, isobutyl silane, propyl silane, 3- (methacryloyloxy) propyl silane, mercapto silane, octadecyl silane, hexadecyl silane, methyl silane, chloropropyl silane, tetramethoxy silane, and polydimethylsiloxane (hydroxyl terminated). 25% to 100% of essential silanes including 50% to 75% of 3- (2, 3-glycidoxy) propyltrimethoxysilane, 25% to 38% of N- (2-aminoethyl) -3-aminopropyltrimethoxysilane, 3% to 25% of perfluorodecyltrimethoxysilane;
further, the catalyst of the 14-50% room temperature curing resin is dibutyl tin dilaurate, and the resin is a net structure with long fluorine-based chains, epoxy groups and silicon-oxygen chains. The long fluorine-based chain can reduce the surface energy of the resin, the epoxy group and the silicon-oxygen chain can interact with the silicon-oxygen bond of the substrate, so that the bonding force between the resin and the substrate is enhanced, and meanwhile, the epoxy group can chemically react with the amino group, so that the mechanical property of the resin is improved.
The 50-85% solvent includes but is not limited to methanol, ethanol, tetrahydrofuran, toluene, ethyl acetate, chloroform.
The 0.25-3% modified nano particles comprise 80-98% nano particles and 2-20% surface modifier;
further, 80% -98% of the 0.25% -3% modified nanoparticles include, but are not limited to, micro/nano-sized silicon dioxide, titanium dioxide, zirconium dioxide, polymer nanoparticles, and the like. 2% -20% of surface modifying agents include but are not limited to heptadecafluorodecyltrimethoxysilane, tridecafluorooctyltriethoxysilane, octadecyltrimethoxysilane, hexadecyltrimethoxysilane.
The invention provides a preparation method of a transparent super-hydrophobic coating, which comprises the following steps:
step (1): an amount of optional silane, 3- (2, 3-glycidoxy) propyltrimethoxysilane and dibutyl tin dilaurate were mixed in a glass flask and stirred for 30min, and then the mixed solution was aged at room temperature for a certain period of time. Then adding a certain amount of perfluorodecyl trimethoxy silane into the solution and stirring for 30min to form chain siloxane. Finally, adding a certain amount of N- (2-aminoethyl) -3-aminopropyltrimethoxysilane into the mixed solution, stirring for ten minutes, and standing to obtain the room-temperature curing resin.
Preferably, the mass ratio of the optional silane, 3- (2, 3-glycidoxy) propyltrimethoxysilane, dibutyl tin dilaurate, perfluorodecyl trimethoxysilane and N- (2-aminoethyl) -3-aminopropyltrimethoxysilane in the step (1) is (50-80): (12-20): (0.2-0.5): (0.1-0.2): (6-10). A further preferred mass ratio is 75: 16: 0.35: 0.15: 8.5.
Step (2): dispersing nano and surface modifier in certain amount of solvent. Stirring for a period of time at room temperature at a certain rotating speed, and carrying out ultrasonic treatment for a certain period of time to obtain a uniformly dispersed nano particle suspension.
Preferably, the mass ratio of the nano particles to the surface modification in the step (2) is 12:1, the stirring time is 1-3h, and the ultrasonic time is 1-2 h.
And (3): and (3) mixing the resin prepared in the step (1) and the nano particle suspension prepared in the step (2) according to a certain mass ratio, and performing ultrasonic treatment for a certain time to obtain a uniform mixed solution.
Preferably, the mass ratio of the resin to the nanoparticle suspension is 1: (1-6) the ultrasonic treatment time is 5-15 min.
And (4): and (4) coating the uniform mixed solution prepared in the step (3) on a substrate by using a spin coating or spray coating method, and standing at room temperature for 24 hours to obtain the super-hydrophobic, transparent and durable coating.
Preferably, the spin coating method: the substrate was placed on a spin coater, spin coater parameters were set at 500rmp,10s and 1000rmp,10s, and the mixed liquid was dropped onto the substrate for spin coating. The spraying method comprises the following steps: placing the prepared mixed solution in a spray gun, keeping the distance between the spray nozzle and the surface of the base material at 20-30cm, the diameter of the spray nozzle at 0.5mm, and the pressure of the spray gun at 0.15MPa, and spraying the mixed solution on the surface of the matrix.
The low surface energy modification of the nanoparticles is realized by grafting and modifying low surface energy molecules on the surfaces of the nanoparticles, and the modified nanoparticles are mixed with the resin with excellent mechanical property solidified at room temperature to obtain uniform dispersion liquid. The dispersion is deposited on the surface of a matrix in a spin coating or spray coating mode, and the super-hydrophobic, transparent and durable coating is prepared. The prepared super-hydrophobic coating has the characteristics of simple method operation, low energy consumption, high efficiency and the like, and has excellent properties of transparency, super-hydrophobicity, good adhesive force, durability, self-cleaning and the like, so that the coating has wide market application prospect.
Drawings
FIG. 1 shows the surface water drop morphology of the superhydrophobic coating of example 8.
FIG. 2 is an SEM image of the surface of the superhydrophobic coating of example 8.
Fig. 3 is a schematic diagram of self-cleaning in example 8.
The specific implementation mode is as follows:
example 1:
step (a): 4.277g of optional silane, 0.945g of 3- (2, 3-glycidoxy) propyltrimethoxysilane, and 0.06g of dibutyltin dilaurate were added in this order to a 25mL beaker and stirred for 30min, and the solution was aged at room temperature for 24 h. Then 0.0034g of perfluorodecyltrimethoxysilane was added to the solution and stirred for 30 min. Subsequently, 0.445g of curing agent N- (2-aminoethyl) -3-aminopropyltrimethoxysilane was added and stirred for 10min to form a stable mixture.
Step (b): in a 50ml flask, 0.9g of SiO2Nanoparticles and 0.072g perfluorodecyltrimethoxysilane were dispersed in 30g ethanol, and the mixture was stirred for 1.5h and sonicated for 1h to give a stable suspension.
Step (c): mixing the mixed liquid prepared in the step (a) and the suspension prepared in the step (b) according to the mass ratio of 1: 1, and carrying out ultrasonic treatment for 5min to form a uniform mixture.
Step (d): and (c) coating the mixture prepared in the step (c) on a substrate in a spin coating or spray coating mode to prepare the super-hydrophobic, transparent and durable coating.
Example 2:
step (a): 4.277g of optional silane, 0.945g of 3- (2, 3-glycidoxy) propyltrimethoxysilane, and 0.06g of dibutyltin dilaurate were added in this order to a 25mL beaker and stirred for 30min, and the solution was aged at room temperature for 24 h. Then 0.0034g of perfluorodecyltrimethoxysilane was added to the solution and stirred for 30 min. Subsequently, 0.445g of curing agent N- (2-aminoethyl) -3-aminopropyltrimethoxysilane was added and stirred for 10min to form a stable mixture.
Step (b): in a 50mL flask, 0.9g of SiO2Nanoparticles and 0.072g perfluorodecyltrimethoxysilane were dispersed in 30g ethanol, and the mixture was stirred for 1.5h and sonicated for 1h to give a stable suspension.
Step (c): mixing the mixed liquid prepared in the step (a) and the suspension prepared in the step (b) according to the mass ratio of 1: 2, and carrying out ultrasonic treatment for 5min to form a uniform mixture.
Step (d): and (c) coating the mixture prepared in the step (c) on a substrate in a spin coating or spray coating mode to prepare the super-hydrophobic, transparent and durable coating.
Example 3:
step (a): 4.277g of optional silane, 0.945g of 3- (2, 3-glycidoxy) propyltrimethoxysilane, and 0.06g of dibutyltin dilaurate were added in this order to a 25mL beaker and stirred for 30min, and the solution was aged at room temperature for 24 h. Then 0.0034g of perfluorodecyltrimethoxysilane was added to the solution and stirred for 30 min. Subsequently, 0.445g of curing agent N- (2-aminoethyl) -3-aminopropyltrimethoxysilane was added and stirred for 10min to form a stable mixture.
Step (b): in a 50mL flask, 0.9g of SiO2Nanoparticles and 0.072g perfluorodecyltrimethoxysilane were dispersed in 30g ethanol, and the mixture was stirred for 1.5h and sonicated for 1h to give a stable suspension.
Step (c): mixing the mixed liquid prepared in the step (a) and the suspension prepared in the step (b) according to the mass ratio of 1: 3, and carrying out ultrasonic treatment for 5min to form a uniform mixture.
Step (d): and (c) coating the mixture prepared in the step (c) on a substrate in a spin coating or spray coating mode to prepare the super-hydrophobic, transparent and durable coating.
Example 4:
step (a): 4.277g of optional silane, 0.945g of 3- (2, 3-glycidoxy) propyltrimethoxysilane, and 0.06g of dibutyltin dilaurate were added in this order to a 25mL beaker and stirred for 30min, and the solution was aged at room temperature for 24 h. Then 0.0034g of perfluorodecyltrimethoxysilane was added to the solution and stirred for 30 min. Subsequently, 0.445g of curing agent N- (2-aminoethyl) -3-aminopropyltrimethoxysilane was added and stirred for 10min to form a stable mixture.
Step (b): in a 50mL flask, 0.9g of SiO2Nanoparticles and 0.072g perfluorodecyltrimethoxysilane were dispersed in 30g ethanol, and the mixture was stirred for 1.5h and sonicated for 1h to give a stable suspension.
Step (c): mixing the mixed liquid prepared in the step (a) and the suspension prepared in the step (b) according to the mass ratio of 1: 4, and carrying out ultrasonic treatment for 5min to form a uniform mixture.
Step (d): and (c) coating the mixture prepared in the step (c) on a substrate in a spin coating or spray coating mode to prepare the super-hydrophobic, transparent and durable coating.
Example 5:
step (a): 4.277g of optional silane, 0.945g of 3- (2, 3-glycidoxy) propyltrimethoxysilane, and 0.06g of dibutyltin dilaurate were added in this order to a 25mL beaker and stirred for 30min, and the solution was aged at room temperature for 24 h. Then 0.0034g of perfluorodecyltrimethoxysilane was added to the solution and stirred for 30 min. Subsequently, 0.445g of curing agent N- (2-aminoethyl) -3-aminopropyltrimethoxysilane was added and stirred for 10min to form a stable mixture.
Step (b): in a 50mL flask, 1.5g of SiO2Dispersing the nano particles and 0.12g of perfluorodecyl trimethoxy silane into 30g of ethanol, stirring the mixture for 1.5h, and carrying out ultrasonic treatment for 1h to obtain the nano-particleTo a stable suspension.
Step (c): mixing the mixed liquid prepared in the step (a) and the suspension prepared in the step (b) according to the mass ratio of 1: 1, and carrying out ultrasonic treatment for 5min to form a uniform mixture.
Step (d): and (c) coating the mixture prepared in the step (c) on a substrate in a spin coating or spray coating mode to prepare the super-hydrophobic, transparent and durable coating.
Example 6:
step (a): 4.277g of optional silane, 0.945g of 3- (2, 3-glycidoxy) propyltrimethoxysilane, and 0.06g of dibutyltin dilaurate were added in this order to a 25mL beaker and stirred for 30min, and the solution was aged at room temperature for 24 h. Then 0.0034g of perfluorodecyltrimethoxysilane was added to the solution and stirred for 30 min. Subsequently, 0.445g of curing agent N- (2-aminoethyl) -3-aminopropyltrimethoxysilane was added and stirred for 10min to form a stable mixture.
Step (b): in a 50mL flask, 0.9g of SiO2Nanoparticles and 0.072g perfluorodecyltrimethoxysilane were dispersed in 30g ethanol, and the mixture was stirred for 1.5h and sonicated for 1h to give a stable suspension.
Step (c): mixing the mixed liquid prepared in the step (a) and the suspension prepared in the step (b) according to the mass ratio of 1: 2, and carrying out ultrasonic treatment for 5min to form a uniform mixture.
Step (d): and (c) coating the mixture prepared in the step (c) on a substrate in a spin coating or spray coating mode to prepare the super-hydrophobic, transparent and durable coating.
Example 7:
step (a): 4.277g of optional silane, 0.945g of 3- (2, 3-glycidoxy) propyltrimethoxysilane, and 0.06g of dibutyltin dilaurate were added in this order to a 25mL beaker and stirred for 30min, and the solution was aged at room temperature for 24 h. Then 0.0034g of perfluorodecyltrimethoxysilane was added to the solution and stirred for 30 min. Subsequently, 0.445g of curing agent N- (2-aminoethyl) -3-aminopropyltrimethoxysilane was added and stirred for 10min to form a stable mixture.
Step (b): at 5In a 0mL flask, 0.9g of SiO2Nanoparticles and 0.072g perfluorodecyltrimethoxysilane were dispersed in 30g ethanol, and the mixture was stirred for 1.5h and sonicated for 1h to give a stable suspension.
Step (c): mixing the mixed liquid prepared in the step (a) and the suspension prepared in the step (b) according to the mass ratio of 1: 3, and carrying out ultrasonic treatment for 5min to form a uniform mixture.
Step (d): and (c) coating the mixture prepared in the step (c) on a substrate in a spin coating or spray coating mode to prepare the super-hydrophobic, transparent and durable coating.
Example 8:
step (a): 4.277g of optional silane, 0.945g of 3- (2, 3-glycidoxy) propyltrimethoxysilane, and 0.06g of dibutyltin dilaurate were added in this order to a 25mL beaker and stirred for 30min, and the solution was aged at room temperature for 24 h. Then 0.0034g of perfluorodecyltrimethoxysilane was added to the solution and stirred for 30 min. Subsequently, 0.445g of curing agent N- (2-aminoethyl) -3-aminopropyltrimethoxysilane was added and stirred for 10min to form a stable mixture.
Step (b): in a 50mL flask, 0.9g of SiO2Nanoparticles and 0.072g perfluorodecyltrimethoxysilane were dispersed in 30g ethanol, and the mixture was stirred for 1.5h and sonicated for 1h to give a stable suspension.
Step (c): mixing the mixed liquid prepared in the step (a) and the suspension prepared in the step (b) according to the mass ratio of 1: 4, and carrying out ultrasonic treatment for 5min to form a uniform mixture.
Step (d): and (c) coating the mixture prepared in the step (c) on a substrate in a spin coating or spray coating mode to prepare the super-hydrophobic, transparent and durable coating.
Example 8 test data
| Serial number | Inspection item | Technical index |
| 1 | Appearance of the product | Even and white |
| 2 | Contact angle | 160.1° |
| 3 | Transmittance (200 ion 800nm) | 93.6％ |
| 4 | Adhesion force | The contact angle was maintained at 140 ° after 200 cycles of the tape application test |
| 5 | Chemical resistance (PH 1,7,14) | After dipping for 40min, the hydrophobic angle of the coating soaked by only the alkaline solution is obviously reduced |
| 6 | Heat resistance | After the heat preservation at 200 ℃ for 4 hours, the hydrophobic angle has no obvious change, and the film turns slightly yellow |
| 7 | Resistance to ultraviolet aging | No significant change in the hydrophobic angle after 7 days of testing according to ASTM D4587 |
| 8 | Impact resistance | The contact angle is kept at 135 DEG after 6000 water drop impact test |
| 9 | Applications of | Can be applied to self-cleaning and oil-water separation |
From the above examples, it can be seen that the super-hydrophobic coating with high durability prepared by the super-hydrophobic coating of the present invention has a coating contact angle of 160.1 °, a high transmittance (93.6), good adhesion, durability to acid, ultraviolet, impact and high temperature, and potential application value. In conclusion, the super-hydrophobic, transparent and durable coating is prepared by a simple process method.
Claims (9)
1. The super-hydrophobic, transparent and durable coating comprises room temperature curing resin, a solvent and modified nanoparticles in the following mass ratio;
the coating comprises 14% -50% of room temperature curing resin, 50% -85% of solvent and 0.25% -3% of modified nanoparticles.
2. The 14-50% of room temperature curing resin comprises 0-75% of optional silane and 25-100% of essential silane;
0-75% of the optional silane in the 14-50% room temperature curing resin comprises one or more of phenyl silane, isobutyl silane, propyl silane, 3- (methacryloyloxy) propyl silane, mercapto silane, octadecyl silane, hexadecyl silane, methyl silane, chloropropyl silane, tetramethoxy silane and polydimethylsiloxane (hydroxyl terminated); 25% to 100% of essential silanes including 50% to 75% of 3- (2, 3-glycidoxy) propyltrimethoxysilane, 25% to 38% of N- (2-aminoethyl) -3-aminopropyltrimethoxysilane, 3% to 25% of perfluorodecyltrimethoxysilane;
the catalyst of the 14-50% room temperature curing resin is dibutyl tin dilaurate, the resin is in a net structure with a long fluoro-group chain, an epoxy group and a silicon-oxygen chain, the long fluoro-group chain can reduce the surface energy of the resin, the epoxy group and the silicon-oxygen chain can interact with a silicon-oxygen bond of a substrate so as to enhance the bonding force of the resin and the substrate, and meanwhile, the epoxy group can chemically react with an amino group so as to improve the mechanical property of the resin.
3. The 50-85% solvent includes but is not limited to methanol, ethanol, tetrahydrofuran, toluene, ethyl acetate, chloroform.
4. The 0.25-3% modified nano particles comprise 80-98% nano particles and 2-20% surface modifier;
80% -98% of the 0.25% -3% modified nanoparticles comprise but are not limited to micron/nano-scale silicon dioxide, titanium dioxide, zirconium dioxide, polymer nanoparticles and the like; 2% -20% of surface modifying agents include but are not limited to heptadecafluorodecyltrimethoxysilane, tridecafluorooctyltriethoxysilane, octadecyltrimethoxysilane, hexadecyltrimethoxysilane.
5. The invention provides a preparation method of a transparent super-hydrophobic coating, which comprises the following steps:
step (1): mixing a certain amount of unnecessary silane, 3- (2, 3-epoxypropoxy) propyl trimethoxy silane and dibutyl tin dilaurate in a glass flask, stirring for 30min, aging the mixed solution at room temperature for a certain time, adding a certain amount of perfluorodecyl trimethoxy silane into the solution, stirring for 30min to form chain siloxane, adding a certain amount of N- (2-aminoethyl) -3-aminopropyl trimethoxy silane into the mixed solution, stirring for ten minutes, and standing to obtain room-temperature curing resin;
step (2): dispersing nano particles and a surface modifier in a certain amount of solvent according to a preset mass ratio, stirring at a certain rotating speed for a period of time at room temperature, and performing ultrasonic treatment for a certain time to obtain a uniformly dispersed nano particle suspension;
and (3): mixing the resin prepared in the step (1) and the nano particle suspension prepared in the step (2) according to a certain mass ratio, and performing ultrasonic treatment for a certain time to obtain a uniform mixed solution;
and (4): and (4) coating the uniform mixed solution prepared in the step (3) on a substrate by using a spin coating or spray coating method, and standing at room temperature for 24 hours to obtain the super-hydrophobic, transparent and durable coating.
6. The method of claim 5, wherein the optional silane, 3- (2, 3-glycidoxy) propyltrimethoxysilane, dibutyl tin dilaurate, perfluorodecyltrimethoxysilane, and N- (2-aminoethyl) -3-aminopropyltrimethoxysilane are present in the amount of (50-80) to (12-20) to (0.2-0.5) to (0.1-0.2) to (6-10) in step (1).
7. The preparation method of the transparent superhydrophobic coating according to claim 5, wherein the mass ratio of the nanoparticles to the surface modification in the step (2) is 12:1, the stirring time is 1-3h, and the ultrasonic time is 1-2 h.
8. The preparation method of the transparent super-hydrophobic coating according to claim 5, characterized in that the mass ratio of the resin to the nanoparticle suspension in the step (3) is 1 (1-6), and the ultrasonic time is 5-15 min.
9. The method for preparing the transparent superhydrophobic coating according to claim 5, wherein the spin coating method in the step (4): placing the substrate on a spin coater, setting the parameters of a spin coater to be 500rmp,10s and 1000rmp,10s, and then dropping the mixed liquid on the substrate for spin coating; the spraying method comprises the following steps: placing the prepared mixed solution in a spray gun, keeping the distance between the spray nozzle and the surface of the base material at 20-30cm, the diameter of the spray nozzle at 0.5mm, and the pressure of the spray gun at 0.15MPa, and spraying the mixed solution on the surface of the matrix.
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Application publication date: 20210105 |
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