CN116218320A - Preparation method of super-hydrophobic self-cleaning aluminum alloy coating - Google Patents

Preparation method of super-hydrophobic self-cleaning aluminum alloy coating Download PDF

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CN116218320A
CN116218320A CN202310298244.1A CN202310298244A CN116218320A CN 116218320 A CN116218320 A CN 116218320A CN 202310298244 A CN202310298244 A CN 202310298244A CN 116218320 A CN116218320 A CN 116218320A
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aluminum alloy
sio
alloy coating
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CN116218320B (en
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王仲民
李家丞
曾庆煜
周达
付俊伟
陈治武
赵茂密
卢照
魏立恭
蒋世伶
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Guangxi Guangxi Academy Of Sciences Aluminum Co ltd
Guangxi Academy of Sciences
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Guangxi Guangxi Academy Of Sciences Aluminum Co ltd
Guangxi Academy of Sciences
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D163/00Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D5/00Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/08Anti-corrosive paints
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
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    • C08K2201/011Nanostructured additives

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Abstract

The invention relates to the technical field of aluminum alloy coatings, and discloses a preparation method of a super-hydrophobic self-cleaning aluminum alloy coating, which utilizes amino and isocyanate SiO of N- (3-aminopropyl) methacrylamide hydrochloride 2 Reacting the isocyanate groups on the surface to obtain acrylamide SiO 2 The introduced acrylamide group and perfluorohexyl ethyl methacrylate, octadecyl acrylate and double-end vinyl polysiloxane are subjected to copolymerization reaction, so that the fluorine-containing organosilicon polymer is grafted to the nano SiO 2 The surface is obtained to obtain the hydrophobic modified nano SiO 2 Finally, the nano SiO is compounded with epoxy resin and coated on the surface of aluminum alloy, and the nano SiO is obtained after heat curing 2 The super-hydrophobic coating compounded with the epoxy resin has a water contact angle of 153.6 degrees at most, and the impact strength of the aluminum alloy coating reaches 15.4kJ/m 2 The coating is not pulverized, does not crack, does not foam, and has excellent corrosion resistance.

Description

Preparation method of super-hydrophobic self-cleaning aluminum alloy coating
Technical Field
The invention relates to the technical field of aluminum alloy coatings, in particular to a preparation method of a super-hydrophobic self-cleaning aluminum alloy coating.
Background
The aluminum alloy has the advantages of low density, light weight, high strength, good electric conduction and thermal conductivity, excellent casting performance and weldability, is widely applied to the fields of transportation, aerospace, mechanical manufacturing and the like, adopts high polymer resin to form a coating on the surface of the aluminum alloy, can endow the aluminum alloy with excellent surface properties such as corrosion resistance, superhydrophobic and the like, and reports on fluorine-containing polyurethane and nano SiO (silicon dioxide) in the literature, namely the preparation of the superhydrophobic coating on the surface of the aluminum alloy and the corrosion resistance of the superhydrophobic coating 2 Under the synergistic effect, a layer of super-hydrophobic coating is successfully prepared on the surface of the aluminum alloy, and the aluminum alloy has excellent corrosion resistance.
The super-hydrophobic coating has a unique super-hydrophobic self-cleaning effect, and has wide application prospects in the fields of metal surface water resistance, rust resistance, outdoor building antifouling and corrosion resistance and the like, for example, patent 202010695661.6, a preparation method of an aluminum alloy surface super-hydrophobic composite coating, discloses that phosphoric acid anodic oxidation treatment is carried out on the aluminum alloy surface; for SiO 2 Carrying out hydrophobic modification treatment, preparing a coating with epoxy resin, fluorine-containing polyurethane and the like, then spraying on the surface of the aluminum alloy, and curing at room temperature to obtain the super-hydrophobic composite coating. The invention aims at preparing hydrophobically modified fluorine-containing organosilicon polymer-based SiO 2 Is compounded with epoxy resin in aluminum alloyThe surface is provided with a super-hydrophobic coating, so that the performances of super-hydrophobic self-cleaning, corrosion resistance, impact resistance and the like of the aluminum alloy surface are improved.
Disclosure of Invention
(one) solving the technical problems
The invention provides a super-hydrophobic self-cleaning aluminum alloy coating, which endows the aluminum alloy coating with excellent super-hydrophobic self-cleaning, corrosion resistance, shock resistance and other properties.
(II) technical scheme
The preparation method of the super-hydrophobic self-cleaning aluminum alloy coating comprises the following steps:
(1) Nano SiO 2 And 2, 4-toluene diisocyanate in toluene solvent to obtain isocyanato SiO 2 Dispersing in reaction solvent, adding N- (3-aminopropyl) methacrylamide hydrochloride, stirring to dissolve, dripping dibutyl tin dilaurate, filtering solvent after reaction, washing the product with ethanol to obtain acrylamido SiO 2
(2) Acrylic amide group SiO 2 Dispersing into methyl isobutyl ketone solvent, adding perfluorohexyl ethyl methacrylate, octadecyl acrylate, double-end vinyl polysiloxane, sodium dodecyl sulfate and OP-10, stirring and emulsifying uniformly, adding azodiisobutyronitrile in nitrogen atmosphere, filtering solvent after reaction, washing the product with distilled water and ethanol to obtain fluorine-containing organosilicon polymer base SiO 2
(3) To the fluorine-containing organosilicon polymer base SiO 2 Adding into emulsion of epoxy resin, ultrasonic dispersing, adding into curing agent methyl hexahydrophthalic anhydride and accelerator 2,4, 6-tri (dimethylamino methyl) phenol, uniformly coating the emulsion on the surface of aluminum alloy, and heating for curing to obtain the super-hydrophobic self-cleaning aluminum alloy coating.
Preferably, the reaction solvent in (1) comprises tetrahydrofuran, acetone, toluene, N-dimethylformamide or ethyl acetate.
Preferably, the isocyanate group SiO in the above (1) 2 The weight ratio of N- (3-aminopropyl) methacrylamide hydrochloride to dibutyltin dilaurate is 1:2-8:0.002-0.006.
Preferably, the reaction temperature is controlled to be 60-80 ℃ and the reaction time is controlled to be 6-18h in the step (1).
Preferably, the acrylamide group SiO in the step (2) 2 The weight ratio of the perfluorohexyl ethyl methacrylate to the octadecyl acrylate to the double-end vinyl polysiloxane is 1:2-10:1.5-6:3-15.
Preferably, the reaction temperature is controlled to be 65-80 ℃ and the reaction time is controlled to be 4-6h in the step (2).
Preferably, the fluorine-containing organosilicon polymer-based SiO in the step (3) 2 And the weight ratio of the epoxy resin is 0.01-0.05:1.
(III) beneficial technical effects
Amino and isocyanato SiO using N- (3-aminopropyl) methacrylamide hydrochloride 2 Reacting the isocyanate groups on the surface to obtain acrylamide SiO 2 The introduced acrylamide group is subjected to copolymerization reaction with perfluorohexyl ethyl methacrylate, octadecyl acrylate and double-end vinyl polysiloxane, so that the hydrophobic fluorine-containing organosilicon polymer is grafted to the nano SiO 2 The surface is obtained to obtain the hydrophobic modified nano SiO 2 Finally, the nano SiO is compounded with epoxy resin and coated on the surface of aluminum alloy, and the nano SiO is obtained after heat curing 2 Super-hydrophobic coating compounded with epoxy resin and hydrophobically modified nano SiO 2 Uniformly dispersed in the coating to form a micro-nano protruding structure, the water contact angle is up to 153.6 degrees, and the impact strength of the aluminum alloy coating is up to 15.4kJ/m 2 The coating is not pulverized, does not crack, does not foam, and has excellent corrosion resistance.
Detailed Description
Example 1
(1) 0.1g of nano SiO 2 And 0.2g of 2, 4-toluene diisocyanate in a toluene solvent to give an isocyanato SiO 2 Weighing 0.1g, dispersing into acetone, adding 0.2g of N- (3-aminopropyl) methacrylamide hydrochloride, stirring and dissolving, dripping 0.2mg of dibutyltin dilaurate, reacting at 60 ℃ for 12 hours, filtering the solvent after the reaction, washing the product with ethanol to obtain acrylamide-based SiO 2
(2) 0.1g of acrylamido SiO 2 Dispersing into methyl isobutyl ketone solvent, adding 0.2g of perfluorohexyl ethyl methacrylate, 0.15g of octadecyl acrylate, 0.3g of double-end vinyl polysiloxane, 0.05g of sodium dodecyl sulfate and 0.1g of OP-10, stirring and emulsifying uniformly, adding 6mg of azodiisobutyronitrile in nitrogen atmosphere, reacting at 70 ℃ for 5h, filtering the solvent after the reaction, washing the product with distilled water and ethanol to obtain fluorine-containing organosilicon polymer base SiO 2
(3) 0.2g of fluorine-containing organosilicon polymer-based SiO 2 Adding into emulsion containing 20g of epoxy resin, adding 10g of curing agent methyl hexahydrophthalic anhydride and 0.12g of accelerator 2,4, 6-tris (dimethylaminomethyl) phenol after ultrasonic dispersion, uniformly coating the emulsion on the surface of the aluminum alloy, and heating and curing to obtain the super-hydrophobic self-cleaning aluminum alloy coating.
Example 2
(1) 0.1g of nano SiO 2 And 0.2g of 2, 4-toluene diisocyanate in a toluene solvent to give an isocyanato SiO 2 Weighing 0.1g of the mixture, redispersing the mixture into N, N-dimethylformamide, adding 0.4g of N- (3-aminopropyl) methacrylamide hydrochloride, stirring and dissolving the mixture, dropwise adding 0.3mg of dibutyltin dilaurate, reacting the mixture at 60 ℃ for 18 hours, filtering the solvent after the reaction, and washing the product by ethanol to obtain acrylamide SiO 2
(2) 0.1g of acrylamido SiO 2 Dispersing into methyl isobutyl ketone solvent, adding 0.4g of perfluorohexyl ethyl methacrylate, 0.2g of octadecyl acrylate, 0.6g of double-end vinyl polysiloxane, 0.05g of sodium dodecyl sulfate and 0.1g of OP-10, stirring and emulsifying uniformly, adding 15mg of azodiisobutyronitrile in nitrogen atmosphere, reacting at 70 ℃ for 6 hours, filtering the solvent after the reaction, washing the product with distilled water and ethanol to obtain fluorine-containing organosilicon polymer base SiO 2
(3) 0.4g of fluorine-containing organosilicon polymer-based SiO 2 Adding into emulsion containing 20g of epoxy resin, adding 10g of curing agent methyl hexahydrophthalic anhydride and 0.12g of accelerator 2,4, 6-tris (dimethylaminomethyl) phenol after ultrasonic dispersionAnd then uniformly coating the emulsion on the surface of the aluminum alloy, and heating and curing to obtain the super-hydrophobic self-cleaning aluminum alloy coating.
Example 3
(1) 0.1g of nano SiO 2 And 0.2g of 2, 4-toluene diisocyanate in a toluene solvent to give an isocyanato SiO 2 Weighing 0.1g, redispersing into ethyl acetate, adding 0.6g of N- (3-aminopropyl) methacrylamide hydrochloride, stirring and dissolving, dripping 0.4mg of dibutyltin dilaurate, reacting at 60 ℃ for 18h, filtering the solvent after the reaction, washing the product with ethanol to obtain acrylamide SiO 2
(2) 0.1g of acrylamido SiO 2 Dispersing into methyl isobutyl ketone solvent, adding 0.8g of perfluorohexyl ethyl methacrylate, 0.4g of octadecyl acrylate, 1.2g of double-end vinyl polysiloxane, 0.05g of sodium dodecyl sulfate and 0.1g of OP-10, stirring and emulsifying uniformly, adding 35mg of azodiisobutyronitrile in nitrogen atmosphere, reacting at 70 ℃ for 4 hours, filtering the solvent after the reaction, washing the product with distilled water and ethanol to obtain fluorine-containing organosilicon polymer base SiO 2
(3) 0.8g of fluorine-containing organosilicon polymer-based SiO 2 Adding into emulsion containing 20g of epoxy resin, adding 10g of curing agent methyl hexahydrophthalic anhydride and 0.12g of accelerator 2,4, 6-tris (dimethylaminomethyl) phenol after ultrasonic dispersion, uniformly coating the emulsion on the surface of the aluminum alloy, and heating and curing to obtain the super-hydrophobic self-cleaning aluminum alloy coating.
Example 4
(1) 0.1g of nano SiO 2 And 0.2g of 2, 4-toluene diisocyanate in a toluene solvent to give an isocyanato SiO 2 Weighing 0.1g, dispersing into toluene, adding 0.8g of N- (3-aminopropyl) methacrylamide hydrochloride, stirring and dissolving, dripping 0.6mg of dibutyltin dilaurate, reacting at 70 ℃ for 18h, filtering the solvent after the reaction, washing the product with ethanol to obtain acrylamide-based SiO 2
(2) 0.1g of acrylamido SiO 2 Dispersing into methyl isobutyl ketone solvent, and adding 1g of perfluoroHexyl ethyl methacrylate, 0.6g of octadecyl acrylate, 1.5g of double-end vinyl polysiloxane, 0.05g of sodium dodecyl sulfate and 0.1g of OP-10, stirring and emulsifying uniformly, adding 50mg of azodiisobutyronitrile in a nitrogen atmosphere, reacting at 75 ℃ for 6 hours, filtering a solvent after the reaction, and washing a product by distilled water and ethanol to obtain the fluorine-containing organosilicon polymer base SiO 2
(3) 1g of a fluorosilicone polymer-based SiO 2 Adding into emulsion containing 20g of epoxy resin, adding 10g of curing agent methyl hexahydrophthalic anhydride and 0.12g of accelerator 2,4, 6-tris (dimethylaminomethyl) phenol after ultrasonic dispersion, uniformly coating the emulsion on the surface of the aluminum alloy, and heating and curing to obtain the super-hydrophobic self-cleaning aluminum alloy coating.
Comparative example 1
(1) 0.2g of nano SiO 2 Adding into emulsion containing 20g of epoxy resin, adding 10g of curing agent methyl hexahydrophthalic anhydride and 0.12g of accelerator 2,4, 6-tris (dimethylaminomethyl) phenol after ultrasonic dispersion, uniformly coating the emulsion on the surface of aluminum alloy, and heating and curing to obtain the aluminum alloy coating.
Comparative example 2
(1) 0.1g of nano SiO 2 And 0.2g of 2, 4-toluene diisocyanate in a toluene solvent to give an isocyanato SiO 2 Weighing 0.1g of the mixture, dispersing the mixture into tetrahydrofuran, adding 0.2g of N- (3-aminopropyl) methacrylamide hydrochloride, stirring and dissolving the mixture, dropwise adding 0.2mg of dibutyltin dilaurate, reacting the mixture at 70 ℃ for 12 hours, filtering the solvent after the reaction, and washing the product by ethanol to obtain acrylamide SiO 2
(2) 0.2g of acrylamido SiO 2 Adding into emulsion containing 20g of epoxy resin, adding 10g of curing agent methyl hexahydrophthalic anhydride and 0.12g of accelerator 2,4, 6-tris (dimethylaminomethyl) phenol after ultrasonic dispersion, uniformly coating the emulsion on the surface of aluminum alloy, and heating and curing to obtain the aluminum alloy coating.
With reference to the method of GB/T30693-2014, a water contact angle tester is used to determine the water contact angle of an aluminum alloy coating.
With reference to the method of GB/T1843-2008, a cantilever beam impact strength tester is adopted to test the impact resistance of the aluminum alloy coating.
The performance of the aluminum alloy media resistance was rated with reference to the method of GB/T1766-2008. The comprehensive grade of the coating film is rated according to the single damage grade in the medium-resistant process of the coating, and is divided into six grades: grade 0 (excellent), grade 1 (good), grade 2 (medium), grade 3 (bad), grade 4 (poor), grade 5 (bad).
Figure BDA0004143937480000061
The maximum water contact angle of the super-hydrophobic self-cleaning aluminum alloy coating reaches 152.2 degrees, and the maximum impact strength reaches 15.4kJ/m 2 The coating is not pulverized, bubble-free, cracking-free and excellent in corrosion resistance.

Claims (7)

1. A preparation method of a super-hydrophobic self-cleaning aluminum alloy coating is characterized by comprising the following steps of: the preparation method comprises the following steps:
(1) Nano SiO 2 And 2, 4-toluene diisocyanate in toluene solvent to obtain isocyanato SiO 2 Dispersing in reaction solvent, adding N- (3-aminopropyl) methacrylamide hydrochloride, stirring to dissolve, dripping dibutyl tin dilaurate, filtering solvent after reaction, washing the product with ethanol to obtain acrylamido SiO 2
(2) Acrylic amide group SiO 2 Dispersing into methyl isobutyl ketone solvent, adding perfluorohexyl ethyl methacrylate, octadecyl acrylate, double-end vinyl polysiloxane, sodium dodecyl sulfate and OP-10, stirring and emulsifying uniformly, adding azodiisobutyronitrile in nitrogen atmosphere, filtering solvent after reaction, washing the product with distilled water and ethanol to obtain fluorine-containing organosilicon polymer base SiO 2
(3) To the fluorine-containing organosilicon polymer base SiO 2 Adding into emulsion of epoxy resin, ultrasonic dispersing, adding into curing agent methyl hexahydrophthalic anhydride and accelerator 2,4, 6-tri (dimethylaminomethyl) phenol, and uniformly coating the emulsionCoating the coating on the surface of the aluminum alloy, and heating and curing to obtain the super-hydrophobic self-cleaning aluminum alloy coating.
2. The method for preparing the superhydrophobic self-cleaning aluminum alloy coating according to claim 1, wherein the method comprises the following steps: the reaction solvent in the step (1) comprises tetrahydrofuran, acetone, toluene, N-dimethylformamide or ethyl acetate.
3. The method for preparing the superhydrophobic self-cleaning aluminum alloy coating according to claim 1, wherein the method comprises the following steps: the isocyanate group SiO of (1) 2 The weight ratio of N- (3-aminopropyl) methacrylamide hydrochloride to dibutyltin dilaurate is 1:2-8:0.002-0.006.
4. The method for preparing the superhydrophobic self-cleaning aluminum alloy coating according to claim 1, wherein the method comprises the following steps: the reaction temperature is controlled to be 60-80 ℃ and the reaction time is controlled to be 6-18h in the step (1).
5. The method for preparing the superhydrophobic self-cleaning aluminum alloy coating according to claim 1, wherein the method comprises the following steps: the acrylamido group SiO of (2) 2 The weight ratio of the perfluorohexyl ethyl methacrylate to the octadecyl acrylate to the double-end vinyl polysiloxane is 1:2-10:1.5-6:3-15.
6. The method for preparing the superhydrophobic self-cleaning aluminum alloy coating according to claim 1, wherein the method comprises the following steps: the reaction temperature is controlled to be 65-80 ℃ and the reaction time is controlled to be 4-6h in the step (2).
7. The method for preparing the superhydrophobic self-cleaning aluminum alloy coating according to claim 1, wherein the method comprises the following steps: the fluorine-containing organosilicon polymer-based SiO in the step (3) 2 And the weight ratio of the epoxy resin is 0.01-0.05:1.
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Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102585245A (en) * 2012-01-13 2012-07-18 中科院广州化学有限公司 High-dispersivity super-amphiphobic microsphere and self-cleaning epoxy resin paint prepared from same
CN103289014A (en) * 2013-06-13 2013-09-11 江苏中恒宠物用品股份有限公司 Synthetic method of stain-resistant cloth surface treating agent
CN110041473A (en) * 2019-04-08 2019-07-23 华南理工大学 A kind of silicon modified aqueous acrylic emulsion and the preparation method and application thereof
CN111732714A (en) * 2020-07-17 2020-10-02 王康 SiO (silicon dioxide)2Epoxy resin super-hydrophobic anticorrosive material modified by polydimethylsiloxane and preparation method thereof
CN112521822A (en) * 2020-12-02 2021-03-19 韦琪燕 Polyacrylate composition, water-based paint and preparation method thereof
CN113388273A (en) * 2021-06-11 2021-09-14 广东轻工职业技术学院 Fluorinated silica nanoparticles and applications
WO2021202269A1 (en) * 2020-04-03 2021-10-07 Sabic Global Technologies, B.V. Dense modified silica with silane compounds and methods of making and using same
CN114292485A (en) * 2022-02-18 2022-04-08 常州大学 Antibacterial adhesion-resistant hydrophobic anti-reflection material and preparation method and application thereof

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102585245A (en) * 2012-01-13 2012-07-18 中科院广州化学有限公司 High-dispersivity super-amphiphobic microsphere and self-cleaning epoxy resin paint prepared from same
CN103289014A (en) * 2013-06-13 2013-09-11 江苏中恒宠物用品股份有限公司 Synthetic method of stain-resistant cloth surface treating agent
CN110041473A (en) * 2019-04-08 2019-07-23 华南理工大学 A kind of silicon modified aqueous acrylic emulsion and the preparation method and application thereof
WO2021202269A1 (en) * 2020-04-03 2021-10-07 Sabic Global Technologies, B.V. Dense modified silica with silane compounds and methods of making and using same
CN111732714A (en) * 2020-07-17 2020-10-02 王康 SiO (silicon dioxide)2Epoxy resin super-hydrophobic anticorrosive material modified by polydimethylsiloxane and preparation method thereof
CN112521822A (en) * 2020-12-02 2021-03-19 韦琪燕 Polyacrylate composition, water-based paint and preparation method thereof
CN113388273A (en) * 2021-06-11 2021-09-14 广东轻工职业技术学院 Fluorinated silica nanoparticles and applications
CN114292485A (en) * 2022-02-18 2022-04-08 常州大学 Antibacterial adhesion-resistant hydrophobic anti-reflection material and preparation method and application thereof

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