CN116478568B - Amphiphilic nano silicon dioxide filler for improving water resistance of water-based paint and preparation method thereof - Google Patents
Amphiphilic nano silicon dioxide filler for improving water resistance of water-based paint and preparation method thereof Download PDFInfo
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 154
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 126
- 239000005543 nano-size silicon particle Substances 0.000 title claims abstract description 58
- 235000012239 silicon dioxide Nutrition 0.000 title claims abstract description 58
- 239000000945 filler Substances 0.000 title claims abstract description 56
- 239000003973 paint Substances 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims abstract description 16
- MSRJTTSHWYDFIU-UHFFFAOYSA-N octyltriethoxysilane Chemical compound CCCCCCCC[Si](OCC)(OCC)OCC MSRJTTSHWYDFIU-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000012188 paraffin wax Substances 0.000 claims abstract description 14
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 8
- 239000002994 raw material Substances 0.000 claims abstract description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 54
- 239000008367 deionised water Substances 0.000 claims description 28
- 229910021641 deionized water Inorganic materials 0.000 claims description 28
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 27
- 238000005406 washing Methods 0.000 claims description 21
- 238000005530 etching Methods 0.000 claims description 19
- 238000010438 heat treatment Methods 0.000 claims description 18
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 18
- 239000000377 silicon dioxide Substances 0.000 claims description 16
- 238000002156 mixing Methods 0.000 claims description 15
- 239000003960 organic solvent Substances 0.000 claims description 12
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 claims description 10
- WOWHHFRSBJGXCM-UHFFFAOYSA-M cetyltrimethylammonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCC[N+](C)(C)C WOWHHFRSBJGXCM-UHFFFAOYSA-M 0.000 claims description 9
- 230000001804 emulsifying effect Effects 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 9
- 238000005303 weighing Methods 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 4
- VBIIFPGSPJYLRR-UHFFFAOYSA-M Stearyltrimethylammonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCCCC[N+](C)(C)C VBIIFPGSPJYLRR-UHFFFAOYSA-M 0.000 claims description 3
- PFKRTWCFCOUBHS-UHFFFAOYSA-N dimethyl(octadecyl)azanium;chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCCCC[NH+](C)C PFKRTWCFCOUBHS-UHFFFAOYSA-N 0.000 claims description 3
- KGOGNDXXUVELIQ-UHFFFAOYSA-N dioctadecylazanium;chloride Chemical compound Cl.CCCCCCCCCCCCCCCCCCNCCCCCCCCCCCCCCCCCC KGOGNDXXUVELIQ-UHFFFAOYSA-N 0.000 claims description 3
- XJWSAJYUBXQQDR-UHFFFAOYSA-M dodecyltrimethylammonium bromide Chemical compound [Br-].CCCCCCCCCCCC[N+](C)(C)C XJWSAJYUBXQQDR-UHFFFAOYSA-M 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 3
- 230000007774 longterm Effects 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 238000003860 storage Methods 0.000 claims description 3
- 238000000576 coating method Methods 0.000 abstract description 15
- 239000011248 coating agent Substances 0.000 abstract description 14
- 238000010276 construction Methods 0.000 abstract description 2
- 238000005260 corrosion Methods 0.000 abstract description 2
- 230000007797 corrosion Effects 0.000 abstract description 2
- 230000001681 protective effect Effects 0.000 abstract description 2
- 238000007711 solidification Methods 0.000 abstract description 2
- 230000008023 solidification Effects 0.000 abstract description 2
- 230000002269 spontaneous effect Effects 0.000 abstract description 2
- 239000002105 nanoparticle Substances 0.000 abstract 2
- 230000000903 blocking effect Effects 0.000 abstract 1
- 238000001914 filtration Methods 0.000 description 12
- 230000005660 hydrophilic surface Effects 0.000 description 7
- 238000004140 cleaning Methods 0.000 description 6
- 239000000839 emulsion Substances 0.000 description 4
- 150000003839 salts Chemical class 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- 230000004888 barrier function Effects 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000007921 spray Substances 0.000 description 3
- 239000011247 coating layer Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 229940057995 liquid paraffin Drugs 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- 229910000975 Carbon steel Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000010962 carbon steel Substances 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000003075 superhydrophobic effect Effects 0.000 description 1
- 239000004094 surface-active agent Substances 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
- 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
- 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
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
-
- 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
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/08—Anti-corrosive paints
Abstract
The invention belongs to the technical field of fillers, and relates to an amphiphilic nano silicon dioxide filler for water-based paint and a preparation method thereof. The amphiphilic nano silicon dioxide filler for improving the water resistance of the water-based paint comprises the following raw materials in parts by mass: 10-15 parts of nano silicon dioxide, 2-4 parts of 3-aminopropyl triethoxysilane, 3-5 parts of n-octyl triethoxysilane, 2-4 parts of emulsifier, 3-5 parts of 52# paraffin and 5-8 parts of etchant. According to the amphiphilic nano particles with spontaneous orientation, the problem that fillers are difficult to disperse in water is solved by utilizing the interfacial characteristic of amphiphilic nano particles, the nano fillers and the water-based paint are mixed for construction, and a blocking layer is spontaneously formed at the interfacial orientation of the coating in the solidification process, so that the hydrophobicity of the water-based paint is substantially improved, the water is not easy to wet, the overall protective performance of the coating is improved, the water resistance and the corrosion resistance of the paint are greatly improved, and the disadvantage of poor water resistance of the water-based paint is overcome.
Description
Technical Field
The invention belongs to the technical field of fillers, and relates to an amphiphilic nano silicon dioxide filler for improving the water resistance of a water-based paint and a preparation method thereof.
Background
With the rapid development of the building industry, the building market share of China is increasing, and the demand for environment-friendly paint is increasing. The water-based coating material occupies most markets of green coatings, but the water-based coating material introduces a surfactant or hydrophilic group in the process of the water-based resin, so that the coating is very easy to wet in a humid environment after construction so as to fall off, and the tolerance and the decoration of the coating are affected. Therefore, along with the improvement of national environmental protection standards and the requirements of people on life quality, the research and the development and the production of a filler for improving the water resistance of the environmental protection water-based paint are urgent.
In recent years, some researches focus on realizing the complementary advantages among different materials by filling functional materials and forming special microstructures on a coating matrix or an interface, wherein lamellar fillers are used in most cases, the water resistance of the water-based paint is improved by improving the barrier property of the water-based paint, but the water-based paint tends to be aggregated and stacked, and poor in dispersibility, so that the paint performance is affected.
Therefore, it is necessary to develop a filler which can be well dispersed in water and at the same time improve the water resistance of the aqueous coating.
Disclosure of Invention
In order to solve the problems, the invention provides the amphiphilic nano silicon dioxide filler for improving the water resistance of the water-based paint and the preparation method thereof, which can improve the stability of the water-based paint and the water resistance of the paint.
In order to achieve the above object, the present invention provides the following technical solutions.
The amphiphilic nano silicon dioxide filler for improving the water resistance of the water-based paint comprises the following raw materials in parts by mass:
10-15 parts of nano silicon dioxide, 2-4 parts of 3-aminopropyl triethoxysilane, 3-5 parts of n-octyl triethoxysilane, 2-4 parts of emulsifier, 3-5 parts of 52# paraffin and 5-8 parts of etchant.
Further, the emulsifier is one or a combination of more of N, N-dimethyl octadecyl amine hydrochloride, dioctadecyl amine hydrochloride, dodecyl trimethyl ammonium bromide, octadecyl trimethyl ammonium chloride and hexadecyl trimethyl ammonium chloride.
Further, the etchant is ammonium fluoride and water according to the weight ratio of 1:10 is adjusted to the ratio.
The preparation method of the amphiphilic nano silica filler for improving the water resistance of the water-based paint comprises the following steps:
Step 1, weighing nano silicon dioxide, dispersing the nano silicon dioxide in 50 parts of ethanol solution, adding 3-aminopropyl triethoxysilane into the solution, mixing and heating the mixture to 80 ℃ for reaction for 12 hours, and respectively washing the prepared product with deionized water and ethanol to obtain hydrophilic nano silicon dioxide particles.
And 2, adding the hydrophilic silica particles prepared in the step 1 into 50 parts of deionized water, adding an emulsifying agent and liquid paraffin, mixing, vibrating and emulsifying for 5min, adding an etching agent into the mixture, etching the surface exposed on one side of the water phase at room temperature for 3h, and washing the obtained sample with an organic solvent to obtain the hydrophilic nano silica particles on one side of the surface.
And 3, weighing the sample prepared in the step 2, dispersing the sample in 50 parts of organic solvent, adding n-octyl triethoxysilane, fully stirring, heating to 80 ℃ in a water bath, reacting for 12 hours, obtaining the amphiphilic nano silica filler with one hydrophilic side and one lipophilic side after the reaction is finished, washing the filler with deionized water and ethanol, drying and grinding to facilitate long-term storage of the sample.
Further, the organic solvent in the step 2 is n-hexane.
Further, the organic solvent in the step3 is toluene.
Compared with the prior art, the invention has the beneficial effects that.
1. The prepared nano-filler single particles are composed of two areas with different components and properties, the areas are obvious, the hydrophilicity and the hydrophobicity of the different areas are opposite, and the composition and the function of the areas can be finely regulated and controlled. Because the structural characteristic particles have unique orientation at the interface, the bi-component amphiphilic particles have more fields of application than the homogeneous structural filler with single performance before, can be used as a solid emulsifier to emulsify oil-water two phases, and can realize the precise regulation and control of the particles to the emulsion interface by regulating the water-oil ratio. Development of amphiphilic particles with spontaneous orientation, utilizing amphiphilic particles to emulsify water and oil phase film forming filler, forming an emulsion mesoscopic container of water-in-water filler, solving the problem of difficult dispersion of filler in water, mixing the filler emulsion with water-based paint, constructing, and solidifying to enable emulsion breaking and releasing filler to spontaneously form a barrier layer at a coating interface, so that the hydrophobicity of the water-based paint is substantially improved, thereby being not easy to be wetted by water, and greatly improving the water resistance and corrosion resistance of the paint.
2. The filler prepared by the invention has amphipathy, is easy to disperse in the water-based paint, can be used by mixing the filler with the water-based paint according to a proportion, and after the water-based paint is constructed and dried, the filler is self-oriented to arrange, and then the hydrophobic side is directed towards the outer side of a coating interface to construct a super-hydrophobic barrier layer, so that the overall protective performance of the coating is synergistically improved, and the disadvantage of poor water resistance of the water-based paint is overcome. Has wider application prospect.
Drawings
The implementation flow of the invention of fig. 1 is shown as a figure.
Detailed Description
The technical solutions of the present invention will be clearly and completely described below in connection with specific embodiments, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The amphiphilic nano silicon dioxide filler for improving the water resistance of the water-based paint comprises the following raw materials in parts by mass: 10-15 parts of nano silicon dioxide, 2-4 parts of 3-aminopropyl triethoxysilane, 3-5 parts of n-octyl triethoxysilane, 2-5 parts of emulsifying agent, 3-5 parts of 52# paraffin and 5-8 parts of etching agent.
Further, the emulsifier is one or a combination of more of N, N-dimethyl octadecyl amine hydrochloride, dioctadecyl amine hydrochloride, dodecyl trimethyl ammonium bromide, octadecyl trimethyl ammonium chloride and hexadecyl trimethyl ammonium chloride.
The preparation method of the amphiphilic nano silica filler for improving the water resistance of the water-based paint comprises the following steps:
Step 1, weighing nano silicon dioxide, dispersing the nano silicon dioxide in 50 parts of ethanol solution, adding 3-aminopropyl triethoxysilane into the solution, mixing and heating the mixture to 80 ℃ for reaction for 12 hours, and respectively washing the prepared product with deionized water and ethanol to obtain hydrophilic nano silicon dioxide particles.
And 2, adding the hydrophilic silica particles prepared in the step 1 into 50 parts of deionized water, adding an emulsifying agent and liquid paraffin, mixing, vibrating and emulsifying for 5min, adding an etching agent into the mixture, etching the surface exposed on one side of the water phase at room temperature for 3h, and washing the obtained sample with an organic solvent to obtain the hydrophilic nano silica particles on one side of the surface.
And 3, weighing the sample prepared in the step 2, dispersing the sample in 50 parts of organic solvent, adding n-octyl triethoxysilane, fully stirring, heating to 80 ℃ in a water bath, reacting for 12 hours, obtaining the amphiphilic nano silica filler with one hydrophilic side and one lipophilic side after the reaction is finished, washing the filler with deionized water and ethanol, drying and grinding to facilitate long-term storage of the sample.
Further, the etchant in the step 2 is ammonium fluoride and water according to the ratio of 1:10 is adjusted to the ratio.
Further, the organic solvent in the step 2 is n-hexane.
Further, the organic solvent in the step3 is toluene.
The invention provides a novel nano filler of a water-based paint, which is synthesized by nano silicon dioxide, 3-aminopropyl triethoxysilane, n-octyl triethoxysilane, an emulsifier, 52# paraffin and an etchant.
Example 1.
The preparation method of the amphiphilic nano silica filler for improving the water resistance of the water-based paint comprises the following steps:
and step 1, dispersing 10 parts of nano silicon dioxide in 50 parts of ethanol, adding 2 parts of 3-aminopropyl triethoxysilane, mixing and heating to 80 ℃ for reaction for 12 hours, washing with deionized water and ethanol, and filtering to obtain the hydrophilic nano silicon dioxide.
And 2, adding the hydrophilic nano silicon dioxide prepared in the step 1 into 50 parts of deionized water, adding 3 parts of molten 52# paraffin, adding 2 parts of cetyltrimethylammonium chloride, fully oscillating and emulsifying for 5min, adding 5 parts of ammonium fluoride solution (10%wt), etching the surface exposed on one side of the water phase for 3h at room temperature, washing with n-hexane after etching, and filtering the product to obtain the nano silicon dioxide with partial hydrophilic surface.
And 3, dispersing the nano silicon dioxide with the hydrophilic surface on one side, which is obtained in the step 2, in 50 parts of toluene, adding 5 parts of n-octyl triethoxysilane, heating to 80 ℃ for reaction for 12 hours, and cleaning with deionized water and ethanol after the reaction to obtain the amphiphilic nano silicon dioxide filler.
The performance was tested.
Example 2.
The preparation method of the amphiphilic nano silica filler for improving the water resistance of the water-based paint comprises the following steps:
And step 1, dispersing 10 parts of nano silicon dioxide in 50 parts of ethanol, adding 3 parts of 3-aminopropyl triethoxysilane, mixing and heating to 80 ℃ for reaction for 12 hours, washing with deionized water and ethanol, and filtering to obtain the hydrophilic nano silicon dioxide.
And 2, adding the hydrophilic nano silicon dioxide prepared in the step 1 into 50 parts of deionized water, adding 3 parts of molten 52# paraffin, adding 2 parts of cetyltrimethylammonium chloride, fully oscillating and emulsifying for 5min, adding 5 parts of ammonium fluoride solution (10%wt), etching the surface exposed on one side of the water phase for 3h at room temperature, washing with n-hexane after etching, and filtering the product to obtain the nano silicon dioxide with partial hydrophilic surface.
And 3, dispersing the nano silicon dioxide with one hydrophilic side obtained in the step 2 in 50 parts of toluene, adding 5 parts of n-octyl triethoxysilane, heating to 80 ℃ for reaction for 12 hours, and cleaning with deionized water and ethanol after the reaction to obtain the amphiphilic nano silicon dioxide filler.
The performance was tested.
Example 3.
The preparation method of the amphiphilic nano silica filler for improving the water resistance of the water-based paint comprises the following steps:
and step 1, dispersing 10 parts of nano silicon dioxide in 50 parts of ethanol, adding 4 parts of 3-aminopropyl triethoxysilane, mixing and heating to 80 ℃ for reaction for 12 hours, washing with deionized water and ethanol, and filtering to obtain the hydrophilic nano silicon dioxide.
And 2, adding the hydrophilic nano silicon dioxide prepared in the step 1 into 50 parts of deionized water, adding 3 parts of molten 52# paraffin, adding 2 parts of cetyltrimethylammonium chloride, fully oscillating and emulsifying for 5min, adding 5 parts of ammonium fluoride solution (10%wt), etching the surface exposed on one side of the water phase for 3h at room temperature, washing with n-hexane after etching, and filtering the product to obtain the nano silicon dioxide with partial hydrophilic surface.
And 3, dispersing the nano silicon dioxide with one hydrophilic side obtained in the step 2 in 50 parts of toluene, adding 5 parts of n-octyl triethoxysilane, heating to 80 ℃ for reaction for 12 hours, and cleaning with deionized water and ethanol after the reaction to obtain the amphiphilic nano silicon dioxide filler.
The performance was tested.
Example 4.
The preparation method of the amphiphilic nano silica filler for improving the water resistance of the water-based paint comprises the following steps:
And step 1, dispersing 10 parts of nano silicon dioxide in 50 parts of ethanol, adding 3 parts of 3-aminopropyl triethoxysilane, mixing and heating to 80 ℃ for reaction for 12 hours, washing with deionized water and ethanol, and filtering to obtain the hydrophilic nano silicon dioxide.
And 2, adding the hydrophilic nano silicon dioxide prepared in the step 1 into 50 parts of deionized water, adding 3 parts of molten 52# paraffin, adding 2 parts of cetyltrimethylammonium chloride, fully oscillating and emulsifying for 5min, adding 5 parts of ammonium fluoride solution (10%wt), etching the surface exposed on one side of the water phase for 3h at room temperature, washing with n-hexane after etching, and filtering the product to obtain the nano silicon dioxide with partial hydrophilic surface.
And 3, dispersing the nano silicon dioxide with one hydrophilic side obtained in the step 2 in 50 parts of toluene, adding 3 parts of n-octyl triethoxysilane, heating to 80 ℃ for reaction for 12 hours, and cleaning with deionized water and ethanol after the reaction to obtain the amphiphilic nano silicon dioxide filler.
The performance was tested.
Example 5.
The preparation method of the amphiphilic nano silica filler for improving the water resistance of the water-based paint comprises the following steps:
and step 1, dispersing 10 parts of nano silicon dioxide in 50 parts of ethanol, adding 2 parts of 3-aminopropyl triethoxysilane, mixing and heating to 80 ℃ for reaction for 12 hours, washing with deionized water and ethanol, and filtering to obtain the hydrophilic nano silicon dioxide.
And step 2, adding the hydrophilic nano silicon dioxide prepared in the step 1 into 50 parts of deionized water, adding 4 parts of molten 52# paraffin, adding 2 parts of cetyltrimethylammonium chloride, fully oscillating and emulsifying for 5min, adding 5 parts of ammonium fluoride solution (10%wt), etching the surface exposed on one side of the water phase for 3h at room temperature, washing with n-hexane after etching, and filtering the product to obtain the nano silicon dioxide with partial hydrophilic surface.
And 3, dispersing the nano silicon dioxide with one hydrophilic side obtained in the step 2 in 50 parts of toluene, adding 5 parts of n-octyl triethoxysilane, heating to 80 ℃ for reaction for 12 hours, and cleaning with deionized water and ethanol after the reaction to obtain the amphiphilic nano silicon dioxide filler.
The performance was tested.
Example 6.
The preparation method of the amphiphilic nano silica filler for improving the water resistance of the water-based paint comprises the following steps:
and step 1, dispersing 10 parts of nano silicon dioxide in 50 parts of ethanol, adding 2 parts of 3-aminopropyl triethoxysilane, mixing and heating to 80 ℃ for reaction for 12 hours, washing with deionized water and ethanol, and filtering to obtain the hydrophilic nano silicon dioxide.
And 2, adding the hydrophilic nano silicon dioxide prepared in the step 1 into 50 parts of deionized water, adding 5 parts of molten 52# paraffin, adding 2 parts of cetyltrimethylammonium chloride, fully oscillating and emulsifying for 5min, adding 5 parts of ammonium fluoride solution (10%wt), etching the surface exposed on one side of the water phase for 3h at room temperature, washing with n-hexane after etching, and filtering the product to obtain the nano silicon dioxide with partial hydrophilic surface.
And 3, dispersing the nano silicon dioxide with one hydrophilic side obtained in the step 2 in 50 parts of toluene, adding 5 parts of n-octyl triethoxysilane, heating to 80 ℃ for reaction for 12 hours, and cleaning with deionized water and ethanol after the reaction to obtain the amphiphilic nano silicon dioxide filler.
The performance was tested.
Examples 1-4 examined the effect on the experiment of the ratio of 3-aminopropyl triethoxysilane to n-octyl triethoxysilane added in part ratios of 2:5, 3:5, 4:5, 1:1, respectively.
Examples 1, 5 and 6 examined the effect of paraffin addition of 3, 4 and 5 parts on the experiment.
The performance test method of the novel nano-filler for improving the water-based paint comprises the following specific steps:
5 parts of the amphiphilic nano filler prepared in the implementation and comparison example, 1000 parts of water-based epoxy resin, 600 parts of resin curing agent and 500 parts of deionized water are mixed, and the mixture is placed into a homogenizer and stirred at 8000r/min for 10 minutes until the mixture is uniform; spraying the stirred mixed paint on a carbon steel sheet by a 5 mm-caliber spray gun, wherein the spraying thickness is controlled to be about 70 microns; and (3) placing the sprayed sample in a shade place, standing for 72 hours, and obtaining a coating sample after complete solidification, and performing performance test.
Table 1 coating performance data.
The neutral salt fog resistant time of the coating prepared by the method is 800-1000h, and the acid salt fog resistant time is 400-600 h; the water contact angle can reach 146 degrees, and the electrochemical impedance value is 1.9 x 10 9-2.1*1010; according to examples 1-4, it can be seen that as the ratio of 3-aminopropyl triethoxysilane to n-octyl triethoxysilane becomes larger, the prepared amphiphilic nano-filler makes the water resistance (acid salt spray resistance time, water contact angle and electrochemical impedance value) of the coating layer become higher and then lower, and according to examples 1, 5 and 6, as the addition amount of paraffin increases, the prepared amphiphilic nano-filler makes the water resistance (acid salt spray resistance time, water contact angle and electrochemical impedance value) of the coating layer become lower.
Claims (5)
1. The preparation method of the amphiphilic nano silica filler for improving the water resistance of the water-based paint is characterized by comprising the following steps of:
Step1, weighing nano silicon dioxide, dispersing the nano silicon dioxide in 50 parts of ethanol solution, adding 3-aminopropyl triethoxysilane into the solution, mixing and heating the mixture to 80 ℃ for reaction for 12 hours, and washing the prepared product with deionized water and ethanol respectively to obtain hydrophilic nano silicon dioxide particles;
Step 2, adding the hydrophilic silica particles prepared in the step 1 into 50 parts of deionized water, adding an emulsifier and molten 52# paraffin, mixing, vibrating and emulsifying for 5min, adding an etchant into the mixture, etching the surface exposed on one side of the water phase at room temperature for 3h, and washing the obtained sample with an organic solvent to obtain hydrophilic nano silica particles on one side of the surface; the etchant is prepared by mixing ammonium fluoride and water in proportion;
Step 3, weighing the sample prepared in the step 2, dispersing the sample in 50 parts of organic solvent, adding n-octyl triethoxysilane, fully stirring, heating to 80 ℃ in a water bath, reacting for 12 hours, obtaining amphiphilic nano silica filler with hydrophilic side and oleophylic side after the reaction is finished, washing the filler with deionized water and ethanol, drying and grinding to facilitate long-term storage of the sample; the filler comprises the following raw materials in parts by mass: 10-15 parts of nano silicon dioxide, 2-4 parts of 3-aminopropyl triethoxysilane, 3-5 parts of n-octyl triethoxysilane, 2-4 parts of emulsifier, 3-5 parts of 52# paraffin and 5-8 parts of etchant.
2. The method for preparing the amphiphilic nano silica filler for improving the water resistance of the water-based paint according to claim 1, wherein the emulsifier is one or a combination of more of N, N-dimethyl octadecyl amine hydrochloride, dioctadecyl amine hydrochloride, dodecyl trimethyl ammonium bromide, octadecyl trimethyl ammonium chloride and hexadecyl trimethyl ammonium chloride.
3. The method for preparing the amphiphilic nano silica filler for improving the water resistance of the water-based paint according to claim 1, wherein the etching agent is ammonium fluoride and water according to the weight ratio of 1:10 is adjusted to the ratio.
4. The method for preparing the amphiphilic nano silica filler for improving the water resistance of the water-based paint according to claim 1, wherein the organic solvent in the step 2 is n-hexane.
5. The method for preparing the amphiphilic nano silica filler for improving the water resistance of the water-based paint according to claim 1, wherein the organic solvent in the step 3 is toluene.
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