CN113913087A - Preparation method of normal-temperature cured wear-resistant anticorrosion super-hydrophobic coating - Google Patents

Preparation method of normal-temperature cured wear-resistant anticorrosion super-hydrophobic coating Download PDF

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CN113913087A
CN113913087A CN202111383029.9A CN202111383029A CN113913087A CN 113913087 A CN113913087 A CN 113913087A CN 202111383029 A CN202111383029 A CN 202111383029A CN 113913087 A CN113913087 A CN 113913087A
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ethyl acetate
spraying
normal
super
mixed solution
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李长全
毛天赐
毛非非
薛智烨
徐国强
厉子昂
王琛
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Jiangsu University of Technology
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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
    • 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
    • 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
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/70—Additives characterised by shape, e.g. fibres, flakes or microspheres
    • 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

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  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Paints Or Removers (AREA)

Abstract

A preparation method of a normal-temperature cured wear-resistant anticorrosion super-hydrophobic coating comprises the following steps: (1) dispersing a multi-walled carbon nanotube and 1H,1H,2H, 2H-perfluorooctyltriethoxysilane in ethyl acetate, and stirring to obtain a mixed solution; (2) epoxy resin, curing agent and SiO2Adding aerogel and ethyl acetate into the mixed solution in proportion; (3) carrying out ultrasonic and stirring on the mixed solution obtained in the step (2) to obtain a spraying liquid; (4) removing oxide layers and other stains on the surface of the steel; (5) the spray gun and the sprayed steel form a 90-degree included angle, the distance between the foremost end of the spray gun and the sprayed steel is 5-50mm, and the spraying time is 30 s; (6) and after spraying, placing the mixture in a ventilated place for drying at normal temperature. The super-hydrophobic coating obtained by the invention has excellent self-cleaning, mechanical and self-repairing performances; successfully constructs a surface micro-nano structure and a bottom layer porous structure group on the surface of the coatingForming a double-layer structure; the spraying mode is used for operation, and the cost is reduced.

Description

Preparation method of normal-temperature cured wear-resistant anticorrosion super-hydrophobic coating
Technical Field
The invention belongs to the technical field of materials, and particularly relates to a material coating technology.
Background
As a novel building mode, most materials can be recycled and degraded, a large amount of garbage can not be generated, and the steel structure assembly type building meets the requirement of green buildings. The steel structure assembly type building has high requirements on corrosion resistance due to the fact that a large amount of steel is adopted, and in order to enable the steel to meet the use requirement of 70 years, the steel needs to be subjected to corrosion resistance treatment.
In the corrosion of steel materials, more than nine times of electrochemical corrosion is considered in the principle except that the corrosion is chemical or physical corrosion in few cases. Three essential factors for electrochemical corrosion to occur: the anode, the cathode and a corrosion medium, water is the most common medium, so the steel corrosion problem can be well solved in a mode of isolating water by the super-hydrophobic coating. However, the biggest problem of the super-hydrophobic coating is that the physical properties are poor and easy to damage.
The invention aims to overcome the defects, and the epoxy resin is widely applied to the preparation of the coating by virtue of the advantages of strong adhesive force, strong mechanical and chemical stability and the like. Can be cured at room temperature in a short time, and is particularly suitable for preparing the room-temperature cured super-hydrophobic coating. However, epoxy resins are brittle after curing and are susceptible to micro-cracks when subjected to impact. The defect can be repaired by adding other materials to the polymer. The nano material has the characteristics of large surface area and high surface energy, and can generate an interface effect when being filled into epoxy resin. The interface effect can enhance the binding force between two phases and improve the strength and toughness of the epoxy resin. Carbon nanotubes are of great interest because of their high electrical conductivity and mechanical properties. They are considered to be ideal reinforcing materials for epoxy resins, enhancing toughness and corrosion resistance. In addition, silica aerogel particles having abrasion resistance and chemical resistance, which can be effectively dispersed in a solvent, improve compatibility with a coating substrate.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a preparation method of a normal-temperature cured wear-resistant anticorrosive super-hydrophobic coating, namely super-hydrophobic EP-SiO2CNTs-POTS coatings were prepared on different substrates by a one-step spray coating and ambient curing technique.
The invention is suitable for corrosion prevention of various steel products and various severe environments, and has excellent protection effect on substrates.
The invention is realized by the following technical scheme.
The invention relates to a preparation method of a normal-temperature cured wear-resistant anticorrosive super-hydrophobic coating.
(1) Modified multi-walled Carbon Nanotubes (CNTs). Dispersing a multi-walled Carbon Nanotube (CNT) and 1H,1H,2H, 2H-Perfluorooctyltriethoxysilane (POTS) in ethyl acetate according to a mass ratio of 1-1.2: 1.2-1: 100, and stirring for 1 hour to obtain a uniformly mixed solution.
(2) Epoxy resin, curing agent and SiO2 Adding aerogel and ethyl acetate into the mixed solution obtained in the step (1) according to the mass ratio of 12:4: 1-3: 100.
(3) And (3) carrying out ultrasonic treatment on the mixed solution obtained in the step (2) for 15-20 minutes, and stirring for 20-30 minutes.
(4) Cleaning before spraying to remove oxide layer and other stains on the surface of the steel.
(5) The spray gun and the sprayed steel form a 90-degree included angle, the distance between the foremost end of the spray gun and the sprayed steel is 5-50mm, and the spraying time is 30 s.
(6) And after the spraying is finished, drying the paint in a ventilation place at normal temperature for 10-12 hours.
Further, the mass ratio of the multi-walled carbon nanotube, 1H,2H, 2H-perfluorooctyltriethoxysilane and ethyl acetate in the step (1) of the invention is preferably 1:1: 100.
Furthermore, the epoxy resin in the step (2) of the invention has a model number of E51, and the curing agent has a model number of D230.
Further, the epoxy resin (EP, E51), the curing agent (D230), and SiO in the step (2) of the present invention2 The mass ratio of aerogel to ethyl acetate is preferably 12:4:1: 100.
The invention has the technical effects that: (1) the coating prepared by the invention combines the advantages of inorganic particles and organic resin, so that the super-hydrophobic coating obtains excellent self-cleaning, mechanical and self-repairing performances; (2) according to the invention, a double-layer structure consisting of a surface micro-nano structure and a bottom layer porous structure is successfully constructed on the surface of the coating; (3) the invention uses a simple spraying mode for operation, and reduces the preparation cost.
Drawings
FIG. 1 is a graph comparing the contact angle before and after abrasion of the coating prepared in example 1 of the present invention. Wherein (a) is EP-SiO2-contact angle of CNTs-POTS coating; (b) is EP-SiO2Contact angle of CNTs-POTS coating after 2000 abrasions (1000 mesh sandpaper with 200g weight).
FIG. 2 is a Bode diagram of the coating of example 1.
FIG. 3 is a Bode plot of a comparative example coating.
FIG. 4 is a Nyquist plot for the coating of example 1.
FIG. 5 is a Nyquist plot for a comparative example coating.
FIG. 6 is a graph comparing the contact angles of comparative example (a) and example 1 (b).
FIG. 7 is a graph comparing the contact angles of example 1 (a), example 2 (b), example 3 (c), example 4 (d), example 5 (e) and comparative example (f).
Detailed Description
The invention will be further illustrated by the following examples.
Example 1.
CNT (0.05 g) and POTS (0.05 g) were dispersed in ethyl acetate (5 g) and stirred for 1 hour. Then the epoxy resin E51, the curing agent D230,SiO2Aerogel and ethyl acetate were added to the above solution in a mass ratio of 12:4:1: 100. To disperse the system uniformly, the mixture was sonicated for 15 minutes and stirred for an additional 30 minutes. Spraying the final solution on the surface of a steel plate and curing for 10 hours at room temperature to form the super-hydrophobic EP-SiO2-CNTs-POTS coating. See table 1.
Example 2.
CNT (0.06 g) and POTS (0.06 g) were dispersed in ethyl acetate (5 g) and stirred for 1 hour. Then epoxy resin E51, curing agent D230 and SiO2Aerogel and ethyl acetate were added to the above solution in a mass ratio of 12:4:1: 100. To disperse the system uniformly, the mixture was sonicated for 15 minutes and stirred for an additional 30 minutes. Spraying the final solution on the surface of a steel plate and curing for 10 hours at room temperature to form the super-hydrophobic EP-SiO2-CNTs-POTS coating. See table 1.
Example 3.
CNT (0.07 g) and POTS (0.07 g) were dispersed in ethyl acetate (5 g) and stirred for 1 hour. Then epoxy resin E51, curing agent D230 and SiO2Aerogel and ethyl acetate were added to the above solution in a mass ratio of 12:4:1: 100. To disperse the system uniformly, the mixture was sonicated for 15 minutes and stirred for an additional 30 minutes. Spraying the final solution on the surface of a steel plate and curing for 10 hours at room temperature to form the super-hydrophobic EP-SiO2-CNTs-POTS coating. See table 1.
Example 4.
CNT (0.05 g) and POTS (0.05 g) were dispersed in ethyl acetate (5 g) and stirred for 1 hour. Then epoxy resin E51, curing agent D230 and SiO2Aerogel and ethyl acetate were added to the above solution in a mass ratio of 15:5:1: 100. To disperse the system uniformly, the mixture was sonicated for 15 minutes and stirred for an additional 30 minutes. Spraying the final solution on the surface of a steel plate and curing for 10 hours at room temperature to form the super-hydrophobic EP-SiO2-CNTs-POTS coating. See table 1.
Example 5.
CNT (0.06 g) and POTS (0.06 g) were dispersed in ethyl acetate (5 g) and stirred for 1 hour. Then oxidizing the epoxyResin E51, curing agent D230, SiO2Aerogel and ethyl acetate were added to the above solution in a mass ratio of 18:6:1: 100. To disperse the system uniformly, the mixture was sonicated for 15 minutes and stirred for an additional 30 minutes. Spraying the final solution on the surface of a steel plate and curing for 10 hours at room temperature to form the super-hydrophobic EP-SiO2-CNTs-POTS coating. See table 1.
Comparative example.
CNT (0.05 g) and POTS (0.05 g) were dispersed in ethyl acetate (5 g) and stirred for 1 hour. Then, epoxy resin E51, curing agent D230 and ethyl acetate were added to the above solution in a mass ratio of 12:4: 100. To disperse the system uniformly, the mixture was sonicated for 15 minutes and stirred for an additional 30 minutes. The final solution was sprayed onto the steel surface and cured at room temperature for 10 hours to form a superhydrophobic EP-CNTs-POTS coating.
Table 1 contact angle, roll angle data for each example
Figure 35656DEST_PATH_IMAGE001
。
EP-SiO of the invention2The abrasion resistance of the-CNTs-POTS coating was evaluated by a wire ball tribometer with 1000 mesh sandpaper loaded with a 200g weight at a controlled rate of 10 cm/min. The WCA and SA comparison of the prepared coating after 1500 times of abrasion is shown in figures 1 (a), (b).
The invention adopts Electrochemical Impedance Spectroscopy (EIS) to further evaluate the long-term corrosion resistance of the prepared coating. FIGS. 2-5 show EP and EP-SiO2Impedance spectra of CNTs-POTS coating after immersion in 3.5wt % NaCl solution 1d, 3d, 5d, 7d, respectively. EP-SiO is clearly visible from FIGS. 2 and 32The 0.01Hz impedance value of the-CNTs-POTS coating was consistently higher than that of the EP coating for 7 days. It is well known that the higher the resistance value at 0.01Hz, the higher the corrosion resistance of the coating will be. Therefore, the super-hydrophobic coating has good long-term corrosion resistance. This can also be observed in correspondence with the Nyquist diagram, EP-SiO in comparison with EP coatings2The semi-circular diameter of the-CNTs-POTS coating can be kept continuously high during the test (FIG. 4, FIG. 5), which is a very important factorIndicating a higher capacitance characteristic.

Claims (4)

1. A preparation method of a normal-temperature cured wear-resistant anticorrosion super-hydrophobic coating is characterized by comprising the following steps:
(1) dispersing a multi-walled carbon nanotube and 1H,1H,2H, 2H-perfluorooctyltriethoxysilane in ethyl acetate according to a mass ratio of 1-1.2: 1.2-1: 100, and stirring for 1 hour to obtain a uniformly mixed solution;
(2) epoxy resin, curing agent and SiO2 Adding aerogel and ethyl acetate into the mixed solution obtained in the step (1) according to the mass ratio of 12:4: 1-3: 100;
(3) carrying out ultrasonic treatment on the mixed solution obtained in the step (2) for 15-20 minutes and stirring for 20-30 minutes to obtain a spraying liquid;
(4) cleaning before spraying to remove oxide layers and other stains on the surface of the steel;
(5) the spray gun and the sprayed steel form a 90-degree included angle, the distance between the foremost end of the spray gun and the sprayed steel is 5-50mm, and the spraying time is 30 s;
(6) and after the spraying is finished, drying the paint in a ventilation place at normal temperature for 10-12 hours.
2. The preparation method of the normal-temperature-cured wear-resistant anticorrosive coating according to claim 1, wherein the epoxy resin in the step (2) is E51 in type and the curing agent is D230 in type.
3. The preparation method of the normal-temperature-curing wear-resistant anticorrosive coating as claimed in claim 1, wherein the mass ratio of the multi-walled carbon nanotube, 1H,2H, 2H-perfluorooctyltriethoxysilane and ethyl acetate in step (1) is 1:1: 100.
4. The method for preparing normal temperature curing wear-resistant anticorrosive coating according to claim 1, characterized in that the epoxy resin, curing agent, SiO in step (2)2 The mass ratio of aerogel to ethyl acetate was 12:4:1: 100.
CN202111383029.9A 2021-11-22 2021-11-22 Preparation method of normal-temperature cured wear-resistant anticorrosion super-hydrophobic coating Pending CN113913087A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116179049A (en) * 2023-02-22 2023-05-30 江苏理工学院 Corrosion-resistant heat-insulating super-hydrophobic coating, and preparation method and application method thereof

Citations (2)

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Publication number Priority date Publication date Assignee Title
CN102492351A (en) * 2011-12-19 2012-06-13 北方涂料工业研究设计院 Conductive super-hydrophobic paint and production method thereof
CN108049236A (en) * 2017-12-14 2018-05-18 中物院成都科学技术发展中心 A kind of packaging super-hydrophobic coat and preparation method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102492351A (en) * 2011-12-19 2012-06-13 北方涂料工业研究设计院 Conductive super-hydrophobic paint and production method thereof
CN108049236A (en) * 2017-12-14 2018-05-18 中物院成都科学技术发展中心 A kind of packaging super-hydrophobic coat and preparation method thereof

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
BIN HAN等: "Durable and anti-corrosion superhydrophobic coating with bistratal structure prepared by ambient curing", 《PROGRESS IN ORGANIC COATINGS》 *
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116179049A (en) * 2023-02-22 2023-05-30 江苏理工学院 Corrosion-resistant heat-insulating super-hydrophobic coating, and preparation method and application method thereof
CN116179049B (en) * 2023-02-22 2023-12-01 江苏理工学院 Corrosion-resistant heat-insulating super-hydrophobic coating, and preparation method and application method thereof

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Application publication date: 20220111