CN112898886A - Anticorrosive anti-icing wear-resistant super-hydrophobic coating and preparation method thereof - Google Patents

Anticorrosive anti-icing wear-resistant super-hydrophobic coating and preparation method thereof Download PDF

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CN112898886A
CN112898886A CN202110155993.XA CN202110155993A CN112898886A CN 112898886 A CN112898886 A CN 112898886A CN 202110155993 A CN202110155993 A CN 202110155993A CN 112898886 A CN112898886 A CN 112898886A
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icing
coating
wear
anticorrosive
preparation
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CN112898886B (en
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胡军
石佳坤
谭远
刘喻波
薛静静
宋卫兵
曹晓飞
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Shaanxi Longlin Nanofiber Materials Technology Co ltd
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Northwestern University
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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
    • C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
    • C09D175/04—Polyurethanes
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • 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
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    • 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
    • C08K2201/002—Physical properties
    • C08K2201/005—Additives being defined by their particle size in general
    • 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 discloses an anticorrosive anti-icing wear-resistant super-hydrophobic coating and a preparation method thereof, belonging to the technical field of metal protection materials and comprising the following steps: modified nano SiO2Preparing particles, preparing a TPU/DMF film forming solution, pretreating a substrate to form a film, and preparing an anticorrosive anti-icing wear-resistant super-hydrophobic coating. The coating prepared by the invention has excellent hydrophobicity, corrosion resistance, anti-icing performance and wear resistance, effectively reduces the safety risk of equipment and components, and prolongs the service life; the preparation method is simple, can realize industrial production and has good market prospect.

Description

Anticorrosive anti-icing wear-resistant super-hydrophobic coating and preparation method thereof
Technical Field
The invention belongs to the technical field of metal protective materials, and particularly relates to an anticorrosive anti-icing wear-resistant super-hydrophobic coating and a preparation method thereof.
Background
The metal material is the most widely used metal material in modern society and plays an important role in human civilization and development. However, metal materials are easy to react with surrounding media to cause metal corrosion, once metal is corroded, the performance of the metal is greatly reduced, and the corrosion protection is a precondition for safe use of various devices, steel members, pipelines and the like, particularly the metal material with the largest amount of steel. The economic loss caused by metal corrosion can reach hundreds of billions of yuan every year, and simultaneously, the method also causes resource waste, delays the technical development and even damages the human health.
In addition, the surface of the metal substrate is easily wetted by water vapor, the hydrophobicity is poor, and in a low-temperature environment, the water vapor is adhered to the surface of the metal and then is frozen, so that certain potential safety hazards are brought to the operation of various devices and components, and various measures for preventing ice and removing snow consume more manpower and material resources. Therefore, the invention provides an anticorrosive anti-icing wear-resistant super-hydrophobic coating and a preparation method thereof.
Disclosure of Invention
The invention provides an anticorrosive anti-icing wear-resistant super-hydrophobic coating and a preparation method thereof, solves the problems of easy corrosion and easy freezing of water vapor on the surface of a metal substrate, and provides a metal surface coating with excellent hydrophobicity and wear resistance.
The invention provides a preparation method of an anticorrosive anti-icing wear-resistant super-hydrophobic coating, which is characterized by comprising the following steps of:
step 1, modifying nano SiO2Preparation of particles
Mixing nano SiO2The particles are immersed into a fluorosilane-absolute ethyl alcohol modified solution for modification at room temperature, and the modified nano SiO is2Drying the particles, and grinding and dispersing;
preparing a film forming solution: dissolving thermoplastic polyurethane elastomer rubber (TPU) in N, N-Dimethylformamide (DMF) to prepare TPU/DMF film-forming solution;
step 2, coating film
Scraping the TPU/DMF film-forming solution in the step 1 on the surface of a pretreated base material, drying, cooling, and repeatedly scraping for many times to form a bottom film layer, namely a TPU coating, on the surface of the metal base material;
step 3, preparing the anticorrosive anti-icing wear-resistant super-hydrophobic coating
Coating the film forming solution prepared in the step 1 on the bottom film layer formed in the step 2 in a scraping manner to obtain a film coating layer; uniformly coating the modified nano SiO prepared in the step 1 on the surface of the coating layer2And (4) preparing a composite layer by using the particles, pressing the composite layer, and drying to obtain the anticorrosive anti-icing wear-resistant super-hydrophobic coating.
Preferably, in step 1, the nano SiO before modification2The particle size of the particles is 10 to 20 nm.
Preferably, in step 1, the nano SiO2The modification time of the particles is 0.5-1 h, and the modified nano SiO2Drying the particles at 90-110 ℃ for 4-6 h.
Preferably, in step 1, the modified nano SiO2The particle size of the particles is 20 to 40 nm.
Preferably, the mass fraction of the fluorosilane in the fluorosilane-absolute ethyl alcohol modified solution is 0.8-1.5 wt%, and the nano SiO is2The mass ratio of the particles to the fluorosilane-absolute ethyl alcohol modified solution is 1: 20 to 25.
Preferably, in the step 1, the concentration of the deposition solution is 0.3-0.35 g/ml; in the step 2, the repeated blade coating times are 3-5.
Preferably, in the step 2, the thickness of the base film layer (TPU coating) is 160-220 μm.
Preferably, in step 3, the pressing specifically comprises: and placing the flat plate on the composite layer, and applying pressure of 10-50N to press for 5-10 min.
Preferably, in step 2, the pretreatment method of the substrate comprises: and (3) polishing the metal base material by using 80-400-mesh sand paper, cleaning the polished metal base material by using distilled water and absolute ethyl alcohol successively, and airing for later use.
The anticorrosive anti-icing wear-resistant super-hydrophobic coating is prepared by the preparation method.
Compared with the prior art, the invention has the beneficial effects that:
(1) the invention coats modified nanometer SiO on the TPU coating2Particles, so that the surface of the base material has a certain chemical composition, and simultaneously, a special micro-nano structure is formed, wherein air cavities in the surface micro-nano structure and-CF on the surface of silicon dioxide3The group enables the coating to have excellent hydrophobicity, the surface solid-liquid contact area is small, the water adhesion is extremely low, and physical separation is formed between a corrosion medium and the coating and between the corrosion medium and a metal substrate, so that the corrosion medium is difficult to contact with metal, and the purpose of corrosion prevention is achieved; the impact liquid drops are bounced off before being frozen, and the freezing time of the liquid drops can be greatly delayed due to the low heat transfer efficiency of the attached liquid drops and the surface, so that the aim of preventing freezing is fulfilled; nano SiO2The particles are half embedded into the surface of the TPU coating, and the TPU coating has certain elasticity, so that external objects firstly touch the nano SiO2The particles can not directly act on the TPU coating, and in addition, the nano SiO2The particles have certain wear resistance, so the wear resistance of the coating is formed by nano SiO2The particles and the TPU coating act synergistically.
(2) The invention adopts fluorosilane-absolute ethyl alcohol modified solution to carry out nano SiO2The particles are subjected to hydrophobic modification to reduce the surface energy, and the concentration is low, the dosage is small, and the environmental pollution is small. The surface of the modified coating obtains excellent hydrophobicity, and has a contact angle of more than 150 degrees and a rolling angle of less than 10 degrees under acidic, neutral and weakly alkaline environments; the anticorrosive anti-icing wear-resistant super-hydrophobic coating prepared by the invention has excellent corrosion resistance, so that the corrosion current density is reduced by 3 orders of magnitude compared with that of a blank metal, the self-corrosion potential is obviously shifted forward, the impedance is increased by more than 300 times, the corrosion rate is effectively delayed, and the corrosion resistance is enhanced; the anticorrosive anti-icing wear-resistant super-hydrophobic coating prepared by the invention has better anti-icing capability, can effectively delay the icing time, and is nearly 3 times longer than that of a bare metal surface.
(3) The anticorrosive anti-icing wear-resistant super-hydrophobic coating prepared by the invention simultaneously meets the anticorrosive anti-icing requirements of the surface of the metal substrate, reduces the safety risk of equipment and components, prolongs the service life, saves manpower, material resources and financial resources because only a common and conventional coating method is adopted, does not need special equipment, and can realize industrial production, thereby obtaining greater economic benefit.
Drawings
FIG. 1 is a flow chart of a preparation process of the anticorrosive, anti-icing and wear-resistant super-hydrophobic coating provided by the invention;
FIG. 2 is the results of the hydrophobicity test of the anti-corrosive, anti-icing, abrasion resistant, superhydrophobic coating of example 3, wherein (a) is the static contact angle and the rolling angle of the coating at different pH; (b) and (c) the contact angle and the rolling angle of water at pH 7 of the coating, respectively;
FIG. 3 is a result of abrasion resistance test of the anti-corrosive, anti-icing, abrasion resistant super-hydrophobic coating prepared in example 3, wherein (a) is a schematic diagram of an abrasion resistance test method; (b) the coating is ground back and forth by 80-mesh sand paper for 100 times to obtain a comparison photograph of the front side (left side) and the back side (right side); (c) and (d) the contact angle and the rolling angle of water after the coating is polished are respectively;
FIG. 4 is an electrochemical test of corrosion resistance of the anticorrosive, anti-icing, wear-resistant and super-hydrophobic coating prepared in example 3 under different corrosion environments, the left side is a polarization curve, and the right side is an impedance spectrum corresponding to the polarization curve; wherein the test environment of (a) and (b) is H with pH 12SO4A solution; (c) the test environment of (d) is 3.5 wt% NaCl solution; (e) the test environment of (f) is NaOH solution with pH 13;
FIG. 5 is an icing-delay test of the anti-icing performance of the anti-corrosion anti-icing wear-resistant super-hydrophobic coating prepared in example 3;
FIG. 6 is photographs (a) and (b) of the coating layer obtained in comparative example 1 before and after polishing with 80-mesh sandpaper, and (c) is a relationship between the concentrations of the deposition solutions and the number of blade coating times in comparative examples 2 to 14;
FIG. 7 is a water droplet morphology on a coating, wherein FIG. 7(a) is a water droplet morphology on a coating prepared by comparative example 15; FIG. 7(b) is the drop morphology on the coating prepared in example 3; FIG. 7(c) is the drop morphology on the coating prepared in comparative example 16; FIG. 7(d) is the drop morphology on the coating prepared in comparative example 17;
FIG. 8 is a schematic diagram showing a mechanism model of the present invention.
Detailed Description
In order to make the technical solutions of the present invention better understood and implemented by those skilled in the art, the present invention is further described below with reference to the following specific embodiments and the accompanying drawings, but the embodiments are not meant to limit the present invention. The following experimental methods and detection methods are conventional methods unless otherwise specified, and the materials and reagents are commercially available.
The invention provides a preparation method of an anticorrosive anti-icing wear-resistant super-hydrophobic coating, which is characterized by comprising the following steps of:
step 1, modifying nano SiO2Preparation of particles
Mixing nano SiO2The particles are immersed into a fluorosilane-absolute ethyl alcohol modified solution for modification at room temperature, and the modified nano SiO is2Drying the particles, and grinding and dispersing;
preparing a film forming solution: dissolving thermoplastic polyurethane elastomer rubber (TPU) in N, N-Dimethylformamide (DMF) to prepare TPU/DMF film-forming solution;
step 2, coating film
Scraping the TPU/DMF film-forming solution in the step 1 on the surface of a pretreated base material, drying, cooling, and repeatedly scraping for many times to form a bottom film layer, namely a TPU coating, on the surface of the metal base material;
step 3, preparing the anticorrosive anti-icing wear-resistant super-hydrophobic coating
Coating the film forming solution prepared in the step 1 on the bottom film layer formed in the step 2 in a scraping manner to obtain a film coating layer; uniformly coating the modified nano SiO prepared in the step 1 on the surface of the coating layer2And (4) preparing a composite layer by using the particles, pressing the composite layer, and drying to obtain the anticorrosive anti-icing wear-resistant super-hydrophobic coating.
The fluorosilane in the fluorosilane-absolute ethyl alcohol modified solution is trimethoxy (1H,1H,2H, 2H-heptadecafluorodecyl) silane or trimethoxy (1H,1H,2H, 2H-tridecafluordecyl) silane; the thermoplastic polyurethane elastomer rubber is TPU 5377A (German Bayer), TPU 1185A (German BASF) and TPU TETON206(Urethane Co)mpounds pty. ltd), TPU 95A (german bayer) and TPU
Figure BDA0002934719560000061
(COIM, italy).
A preparation method of the anticorrosive, anti-icing and wear-resistant super-hydrophobic coating is given by taking 45# steel (50X 80mm) as a metal substrate:
example 1
A preparation method of an anticorrosive, anti-icing and wear-resistant super-hydrophobic coating is shown in figure 1 and comprises the following steps:
step 1, modifying nano SiO2Preparation of particles: 1g of nano SiO with the grain diameter of 10nm2The particles are immersed into a modified solution of 20g of 0.8 wt% of trimethoxy (1H,1H,2H, 2H-heptadecafluorodecyl) silane-absolute ethyl alcohol and stirred at room temperature, after 0.5H of modification, the modified nano SiO is2Drying the particles in an oven at 90 deg.C for 6h, grinding and dispersing to obtain modified nanometer SiO with particle diameter of 20nm2Particles;
step 2, preparing a TPU/DMF film forming solution: dissolving thermoplastic polyurethane elastomer rubber (TPU 5377A) in N, N-Dimethylformamide (DMF) to prepare TPU/DMF film forming solution with the concentration of 0.35 g/ml;
step 3, pretreatment of the base material: polishing 45# steel (50 multiplied by 80mm) by using 80-mesh abrasive paper, cleaning the polished metal base material by using distilled water and absolute ethyl alcohol in sequence, and airing for later use;
step 4, coating a film on a base material: taking 2ml of the TPU/DMF film forming solution obtained in the step 2, carrying out blade coating on the 45# steel processed in the step 3 by using a scraper to form a film, drying, taking out, cooling, carrying out blade coating again, repeating the blade coating for 3 times, and forming a TPU layer with the thickness of 160 mu m on the surface of the 45# steel;
step 5, preparing the anticorrosive anti-icing wear-resistant super-hydrophobic coating: coating a TPU/DMF film forming solution prepared in the step 2 on the TPU layer formed on the surface of the No. 445 steel in a scraping way, and then immediately and uniformly coating the modified nano SiO prepared in the step 1 on the surface of the TPU film forming solution2The particles are scraped by a scraper and covered by a flat plate with nano SiO2On a film of the particles and compacted under a pressure of 10N for 10min, after which it is oven-dried at 100 ℃Drying, cooling and removing excessive SiO on the surface2And (3) granules.
Example 2
A preparation method of an anticorrosive, anti-icing and wear-resistant super-hydrophobic coating is shown in figure 1 and comprises the following steps:
step 1, modifying nano SiO2Preparation of particles: 1g of nano SiO with the grain diameter of 20nm2Immersing the particles into a modified solution of 25g of 1.5 wt% of trimethoxy (1H,1H,2H, 2H-heptadecafluorodecyl) silane-absolute ethyl alcohol, stirring at room temperature, modifying for 1H, and then modifying the modified nano SiO2Drying the particles in an oven at 110 deg.C for 4h, grinding and dispersing to obtain modified nanometer SiO with particle diameter of 40nm2Particles;
step 2, preparing a TPU/DMF film forming solution: dissolving thermoplastic polyurethane elastomer rubber (TPU 5377A) in N, N-Dimethylformamide (DMF) to prepare TPU/DMF film forming solution with the concentration of 0.3 g/ml;
step 3, pretreatment of the base material: grinding 45# steel (50 multiplied by 80mm) by using 400-mesh sand paper, cleaning the ground metal base material by using distilled water and absolute ethyl alcohol in sequence, and airing for later use;
step 4, coating a film on a base material: taking 2ml of the TPU/DMF film-forming solution obtained in the step 2, carrying out blade coating on the 45# steel processed in the step 3 by using a scraper to form a film, drying, taking out, cooling, carrying out blade coating again, repeating the blade coating for 5 times, and forming a TPU layer with the thickness of about 220 microns on the surface of the 45# steel;
step 5, preparing the anticorrosive anti-icing wear-resistant super-hydrophobic coating: coating a TPU/DMF film forming solution prepared in the step 2 on the TPU layer formed on the surface of the No. 445 steel in a scraping way, and then immediately and uniformly coating the modified nano SiO prepared in the step 1 on the surface of the TPU film forming solution2The particles are scraped by a scraper and covered by a flat plate with nano SiO2Coating the particles, compacting under 50N pressure for 5min, drying in 100 deg.C oven, cooling, and removing excessive SiO on the surface2And (3) granules.
Example 3
A preparation method of an anticorrosive, anti-icing and wear-resistant super-hydrophobic coating is shown in figure 1 and comprises the following steps:
step 1, modifying nano SiO2Preparation of particles: 1g of nano SiO with the grain diameter of 15nm2The particles are immersed into 20g of 1.0 wt% of modified solution of trimethoxy (1H,1H,2H, 2H-heptadecafluorodecyl) silane-absolute ethyl alcohol and stirred at room temperature, after modification is carried out for 0.5H, the modified nano SiO is obtained2Drying the particles in an oven at 100 deg.C for 5h, grinding and dispersing to obtain modified nanometer SiO with particle diameter of 30nm2Particles;
step 2, preparing a TPU/DMF film forming solution: dissolving thermoplastic polyurethane elastomer rubber (TPU 5377A) in N, N-Dimethylformamide (DMF) to prepare TPU/DMF film forming solution with the concentration of 0.3 g/ml;
step 3, pretreatment of the base material: polishing 45# steel (50 multiplied by 80mm) by using 80-mesh abrasive paper, cleaning the polished metal base material by using distilled water and absolute ethyl alcohol in sequence, and airing for later use;
step 4, coating a film on a base material: taking 2ml of the TPU/DMF film-forming solution obtained in the step 2, carrying out blade coating and forming on the 45# steel processed in the step 3 by using a scraper, drying, taking out, cooling, carrying out blade coating again, repeating the blade coating for 4 times, and forming a TPU layer with the thickness of about 175 microns on the surface of the 45# steel;
step 5, preparing the anticorrosive anti-icing wear-resistant super-hydrophobic coating: coating a TPU/DMF film forming solution prepared in the step 2 on the TPU layer formed on the surface of the No. 445 steel in a scraping way, and then immediately and uniformly coating the modified nano SiO prepared in the step 1 on the surface of the TPU film forming solution2The particles are scraped by a scraper and covered by a flat plate with nano SiO2Coating the particles, compacting under 30N pressure for 5min, drying in oven at 100 deg.C, cooling, and removing excessive SiO on the surface2And (3) granules.
The performances of the anticorrosive, anti-icing and wear-resistant super-hydrophobic coatings prepared in the above embodiments 1 to 3 are similar, and the following embodiment 3 is taken as an example only, and the comprehensive test of various performance indexes is performed, and the results are as follows:
1) analyzing the hydrophobicity of the anticorrosive anti-icing wear-resistant super-hydrophobic coating: FIG. 2 is the results of the hydrophobicity test of the anti-corrosive, anti-icing, abrasion resistant, superhydrophobic coating of example 3, wherein (a) is the static contact angle and the rolling angle of the coating at different pH; (b) and (c) the contact angle and the rolling angle of water at pH 7 of the coating, respectively, it can be seen that the coating of the present invention has a contact angle of 150 ° or more and a rolling angle of 10 ° or less in acidic, neutral and weakly alkaline environments.
2) Analyzing the wear resistance of the anticorrosive, anti-icing and wear-resistant super-hydrophobic coating: FIG. 3 is a result of abrasion resistance test of the anti-corrosive, anti-icing, abrasion resistant super-hydrophobic coating prepared in example 3, wherein (a) is a schematic diagram of an abrasion resistance test method; (b) the coating is ground back and forth by 80-mesh sand paper for 100 times to obtain a comparison photograph of the front side (left side) and the back side (right side); (c) and (d) the contact angle and the rolling angle of water after the coating is polished are respectively; the invention realizes the adhesion of the metal substrate and the anticorrosive anti-icing wear-resistant super-hydrophobic coating by the TPU, and uses the modified SiO2To construct a surface nano-scale micro-rough structure due to TPU and SiO2The coating prepared in example 3 has certain abrasion resistance and a firm TPU surface microstructure formed after pressurization and heating, so that the reduction degree of the roughness of the surface and the loss of low surface energy components of the coating are limited after the coating is abraded by 80-mesh sand paper, the loss of hydrophobic property is less, and the contact angle and the rolling angle of the coating prepared in example 3 are not greatly changed after the coating is abraded by the sand paper as shown in figures 3(c) and (d).
3) The corrosion resistance and the freezing resistance of the anticorrosive anti-icing wear-resistant super-hydrophobic coating in different corrosion environments are analyzed: FIG. 4 is an electrochemical test of corrosion resistance of the anticorrosive, anti-icing, wear-resistant and super-hydrophobic coating prepared in example 3 under different corrosion environments, the left side is a polarization curve, and the right side is an impedance spectrum corresponding to the polarization curve; wherein the test environment of (a) and (b) is H with pH 12SO4A solution; (c) the test environment of (d) is 3.5 wt% NaCl solution; (e) the test environment of (f) is NaOH solution with pH 13; as can be seen from fig. 4, the corrosion-resistant, anti-icing and wear-resistant super-hydrophobic coating prepared in embodiment 3 of the present invention reduces the corrosion current density by 3 orders of magnitude compared with that of the blank metal, has an obviously forward shift from the corrosion potential, increases the impedance by more than 300 times, effectively delays the corrosion rate, enhances the corrosion resistance, and can effectively protect the metal substrate even if the coating is worn; as can be seen from FIG. 5, the anticorrosive, anti-icing and wear-resistant super-hydrophobic coating prepared in example 3 can effectively delay the icing time, and is nearly 3 times longer than that of a bare metal surface.
In order to further illustrate the effect of the invention, the invention is also provided with a comparative example which is concretely as follows:
comparative example 1
A preparation method of an anticorrosive, anti-icing and wear-resistant super-hydrophobic coating comprises the following steps:
step 1, modifying nano SiO2Preparation of particles: 1g of nano SiO with the grain diameter of 15nm2The particles are immersed into 20g of 1.0 wt% of modified solution of trimethoxy (1H,1H,2H, 2H-heptadecafluorodecyl) silane-absolute ethyl alcohol and stirred at room temperature, after modification is carried out for 0.5H, the modified nano SiO is obtained2Drying the particles in an oven at 100 deg.C for 5h, grinding and dispersing to obtain modified nanometer SiO with particle diameter of 30nm2Particles;
step 2, preparing a TPU/DMF film forming solution: dissolving thermoplastic polyurethane elastomer rubber (TPU 5377A) in N, N-dimethylformamide to prepare TPU/DMF film forming liquid with the concentration of 0.1g/ml respectively;
step 3, pretreatment of the base material: polishing 45# steel (50 multiplied by 80mm) by using 80-mesh abrasive paper, cleaning the polished metal base material by using distilled water and absolute ethyl alcohol in sequence, and airing for later use;
step 4, coating a film on a base material: taking 2ml of the TPU/DMF film forming solution in the step 2, carrying out blade coating on the 45# steel processed in the step 3 by using a scraper to form a mold, drying, taking out, cooling, carrying out blade coating again, repeating for 1 time, and forming a TPU layer on the surface of the 45# steel;
step 5, preparing the anticorrosive anti-icing wear-resistant super-hydrophobic coating: coating a TPU/DMF film forming solution prepared in the step 2 on the TPU layer formed on the surface of the No. 445 steel in a scraping way, and then immediately and uniformly coating the modified nano SiO prepared in the step 1 on the surface of the TPU film forming solution2The particles are scraped by a scraper and covered by a flat plate with nano SiO2Coating the particles, compacting under 30N pressure for 5min, drying in oven at 100 deg.C, cooling, and removing excessive SiO on the surface2And (3) granules.
Comparative example 2
A preparation method of an anticorrosive, anti-icing and wear-resistant super-hydrophobic coating comprises the following steps:
the number of repeated drawdowns in step 4 of comparative example 1 was set to 2, and the remaining parameters were unchanged.
Comparative example 3
A preparation method of an anticorrosive, anti-icing and wear-resistant super-hydrophobic coating comprises the following steps:
the number of repeated drawdowns in step 4 of comparative example 1 was set to 3, and the remaining parameters were unchanged.
Comparative example 4
A preparation method of an anticorrosive, anti-icing and wear-resistant super-hydrophobic coating comprises the following steps:
the number of repeated drawdowns in step 4 of comparative example 1 was set to 4, and the remaining parameters were unchanged.
Comparative example 5
A preparation method of an anticorrosive, anti-icing and wear-resistant super-hydrophobic coating comprises the following steps:
the number of repeated drawing in step 4 of comparative example 1 was set to 5, and the remaining parameters were unchanged.
Comparative example 6
A preparation method of an anticorrosive, anti-icing and wear-resistant super-hydrophobic coating comprises the following steps:
the concentration of the TPU/DMF film formation solution in step 2 of comparative example 1 was set to 0.2g/ml, and the number of repeated blade coating in step 4 was set to 1, with the remaining parameters being unchanged.
Comparative example 7
A preparation method of an anticorrosive, anti-icing and wear-resistant super-hydrophobic coating comprises the following steps:
the concentration of the TPU/DMF film formation solution in step 2 of comparative example 1 was set to 0.2g/ml, and the number of repeated blade coating in step 4 was set to 2 times, with the remaining parameters being unchanged.
Comparative example 8
A preparation method of an anticorrosive, anti-icing and wear-resistant super-hydrophobic coating comprises the following steps:
the concentration of the TPU/DMF film forming solution in step 2 of comparative example 1 was 0.2g/ml, and the number of repeated blade coating in step 4 was set to 3 times, with the remaining parameters being unchanged.
Comparative example 9
A preparation method of an anticorrosive, anti-icing and wear-resistant super-hydrophobic coating comprises the following steps:
the concentration of the TPU/DMF film formation solution in step 2 of comparative example 1 was set to 0.2g/ml, and the number of repeated blade coating in step 4 was set to 4 times, with the remaining parameters being unchanged.
Comparative example 10
A preparation method of an anticorrosive, anti-icing and wear-resistant super-hydrophobic coating comprises the following steps:
the concentration of the TPU/DMF film formation solution in step 2 of comparative example 1 was set to 0.2g/ml, and the number of repeated blade coating in step 4 was set to 5 times, with the remaining parameters being unchanged.
Comparative example 11
A preparation method of an anticorrosive, anti-icing and wear-resistant super-hydrophobic coating comprises the following steps:
the concentration of the TPU/DMF film formation solution in step 2 of comparative example 1 was set to 0.3g/ml, and the number of repeated blade coating in step 4 was set to 1, with the remaining parameters being unchanged.
Comparative example 12
A preparation method of an anticorrosive, anti-icing and wear-resistant super-hydrophobic coating comprises the following steps:
the concentration of the TPU/DMF film formation solution in step 2 of comparative example 1 was set to 0.3g/ml, and the number of repeated blade coating in step 4 was set to 2 times, with the remaining parameters being unchanged.
Comparative example 13
A preparation method of an anticorrosive, anti-icing and wear-resistant super-hydrophobic coating comprises the following steps:
the concentration of the TPU/DMF film formation solution in step 2 of comparative example 1 was set to 0.3g/ml, and the number of repeated blade coating in step 4 was set to 3 times, with the remaining parameters being unchanged.
Comparative example 14
A preparation method of an anticorrosive, anti-icing and wear-resistant super-hydrophobic coating comprises the following steps:
the concentration of the TPU/DMF film formation solution in step 2 of comparative example 1 was set to 0.4g/ml, with the remaining parameters being unchanged.
The anticorrosive, anti-icing and wear-resistant super-hydrophobic coatings prepared in the example 3 and the comparative examples 1 to 14 are respectively tested, and the results are analyzed as follows: FIG. 6 is photographs (a) and (b) of the coating layer obtained in comparative example 2 before and after polishing with 80-mesh sandpaper, and (c) is a relationship between the concentrations of the deposition solutions and the number of blade coating times in comparative examples 1 to 13; as can be seen from FIGS. 6(a) and (b), the coating thickness was small due to the low concentration of the deposition solution (0.1g/ml) and the small number of coating times, and the coating was inferior in abrasion resistance and easily broken. As can be seen from the relationship between the concentration of the deposition solution and the number of blade coating times in FIG. 6(c), 0.1g/ml of the deposition solution is too thin, and the number of coating times is significantly increased if a TPU layer with a proper thickness is achieved; on the other hand, the deposition solution of 0.4g/ml is too viscous to be applied by blade coating, and therefore, it is preferable to control the concentration of the deposition solution to 0.3 g/ml.
Comparative example 15
A preparation method of an anticorrosive, anti-icing and wear-resistant super-hydrophobic coating is shown in figure 1 and comprises the following steps:
step 1, modifying nano SiO2Preparation of particles: 1g of nano SiO2 particles with the particle size of 15nm are immersed into 20g of 0.5 wt% of modified solution of trimethoxy (1H,1H,2H, 2H-heptadecafluorodecyl) silane-absolute ethyl alcohol and stirred at room temperature, after modification is carried out for 0.5H, the modified nano SiO is2Drying the particles at 100 deg.C for 5h, grinding and dispersing to obtain modified nanometer SiO with particle diameter of 30nm2Particles;
step 2, preparing a TPU/DMF film forming solution: dissolving thermoplastic polyurethane elastomer rubber (TPU 5377A) in N, N-dimethylformamide to prepare TPU/DMF film forming solution with the concentration of 0.3 g/ml;
step 3, pretreatment of the base material: polishing 45# steel (50 multiplied by 80mm) by using 80-mesh abrasive paper, cleaning the polished metal base material by using distilled water and absolute ethyl alcohol in sequence, and airing for later use;
step 4, coating a film on a base material: taking 2ml of the TPU/DMF film forming solution in the step 2, carrying out blade coating and forming on the 45# steel processed in the step 3 by using a scraper, drying, taking out, cooling, carrying out blade coating again, repeating the blade coating for 4 times, and forming a TPU layer with the thickness of 200 microns on the surface of the 45# steel;
step 5, preparing the anticorrosive anti-icing wear-resistant super-hydrophobic coating: coating a TPU/DMF film forming solution prepared in the step 2 on the TPU layer formed on the surface of the No. 445 steel in a scraping way, and then immediately and uniformly coating the modified nano SiO prepared in the step 1 on the surface of the TPU film forming solution2The particles are scraped by a scraper and covered by a flat plate with nano SiO2Coating the particles, compacting under 30N pressure for 5min, drying in oven at 100 deg.C, cooling, and removing excessive SiO on the surface2And (3) granules.
Comparative example 16
A preparation method of an anticorrosive, anti-icing and wear-resistant super-hydrophobic coating is shown in figure 1 and comprises the following steps:
step 1, modifying nano SiO2Preparation of particles: 1g of nano SiO with the grain diameter of 15nm2The particles are immersed into a modified solution of 20g of 1.5 wt% of trimethoxy (1H,1H,2H, 2H-heptadecafluorodecyl) silane-absolute ethyl alcohol and stirred at room temperature, after 0.5H of modification, the modified nano SiO is obtained2Drying the particles at 120 deg.C for 5h, grinding and dispersing to obtain modified nanometer SiO with particle diameter of 30nm2Particles;
step 2, preparing a TPU/DMF film forming solution: dissolving thermoplastic polyurethane elastomer rubber (TPU 5377A) in N, N-dimethylformamide to prepare TPU/DMF film forming solution with the concentration of 0.3 g/ml;
step 3, pretreatment of the base material: polishing 45# steel (50 multiplied by 80mm) by using 80-mesh abrasive paper, cleaning the polished metal base material by using distilled water and absolute ethyl alcohol in sequence, and airing for later use;
step 4, coating a film on a base material: taking 2ml of the TPU/DMF film forming solution in the step 2, carrying out blade coating and forming on the 45# steel processed in the step 3 by using a scraper, drying, taking out, cooling, carrying out blade coating again, repeating the blade coating for 4 times, and forming a TPU layer with the thickness of 200 microns on the surface of the 45# steel;
step 5, preparing the anticorrosive anti-icing wear-resistant super-hydrophobic coating: coating a TPU/DMF film forming solution prepared in the step 2 on the TPU layer formed on the surface of the No. 445 steel in a scraping way, and then immediately and uniformly coating the modified nano SiO prepared in the step 1 on the surface of the TPU film forming solution2The particles are scraped by a scraper and covered by a flat plate with nano SiO2Coating the particles, compacting under 30N pressure for 5min, drying in oven at 100 deg.C, cooling, and removing excessive SiO on the surface2And (3) granules.
Comparative example 17
A preparation method of an anticorrosive, anti-icing and wear-resistant super-hydrophobic coating comprises the following steps:
step 1, modifying nano SiO2Preparation of particles: 1g of nano SiO with the grain diameter of 15nm2The particles are immersed into a modified solution of 20g of 1.5 wt% of trimethoxy (1H,1H,2H, 2H-heptadecafluorodecyl) silane-absolute ethyl alcohol and stirred at room temperature, after 0.5H of modification, the modified nano SiO is obtained2Drying the particles at 120 deg.C for 6h, grinding and dispersing to obtain modified nanometer SiO with particle diameter of 30nm2Particles;
step 2, preparing a TPU/DMF film forming solution: dissolving thermoplastic polyurethane elastomer rubber (TPU 5377A) in N, N-dimethylformamide to prepare TPU/DMF film forming solution with the concentration of 0.3 g/ml;
step 3, pretreatment of the base material: polishing 45# steel (50 multiplied by 80mm) by using 80-mesh abrasive paper, cleaning the polished metal base material by using distilled water and absolute ethyl alcohol in sequence, and airing for later use;
step 4, coating a film on a base material: taking 2ml of the TPU/DMF film forming solution in the step 2, carrying out blade coating and forming on the 45# steel processed in the step 3 by using a scraper, drying, taking out, cooling, carrying out blade coating again, repeating the blade coating for 4 times, and forming a TPU layer with the thickness of 200 microns on the surface of the 45# steel;
step 5, preparing the anticorrosive anti-icing wear-resistant super-hydrophobic coating: coating a TPU/DMF film forming solution prepared in the step 2 on the TPU layer formed on the surface of the No. 445 steel in a scraping way, and then immediately and uniformly coating the modified nano SiO prepared in the step 1 on the surface of the TPU film forming solution2The particles are scraped by a scraper and covered by a flat plate with nano SiO2Coating the particles, compacting under 30N pressure for 5min, drying in oven at 100 deg.C, cooling, and removing excessive SiO on the surface2And (3) granules.
The hydrophobicity of the anticorrosive, anti-icing and wear-resistant super-hydrophobic coatings prepared in the example 3 and the comparative examples 15 to 17 is compared, and the results are analyzed as follows: FIG. 7 is a water droplet morphology on a coating, wherein FIG. 7(a) is a water droplet morphology on a coating prepared by comparative example 15; FIG. 7(b) is the drop morphology on the coating prepared in example 3; FIG. 7(c) is the drop morphology on the coating prepared in comparative example 16; FIG. 7(d) shows water on the coating prepared in comparative example 17Droplet morphology. As is clear from FIG. 7(a), SiO was observed due to the low concentration of the 0.5 wt% modifying solution2The particle modification effect is poor, so that the surface of the coating is hydrophilic; as shown in FIG. 7(c), the hydrophobic effect was good after modification with 1.5 wt% of the modifying solution, but SiO was found to be good due to the high drying temperature2The particles become coarse, resulting in non-uniformity of the coating surface; as shown in FIG. 7(d), when the modification was carried out by using the same 1.5 wt% modifying solution and the drying time was prolonged to 6 hours, SiO was observed2The particles lose hydrophobicity; as shown in FIG. 7(b), SiO prepared in example 3 (concentration of the modifying solution: 1.0 wt%, drying temperature: 100 ℃ C., drying time: 5 hours)2The particle size is uniform, and the hydrophobic performance of the coating is excellent.
According to the analysis result, the modified nano SiO is coated on the TPU coating2The particles enable the surface of the base material to have a certain chemical composition, and meanwhile, a special micro-nano structure (as shown in figure 8) is formed, the coating has excellent hydrophobicity due to air pockets in the surface micro-nano structure and-CF 3 groups on the surface of silicon dioxide, the surface solid-liquid contact area is small, the water adhesion is extremely low, physical barriers are formed among corrosion media, the coating and a metal substrate, and the corrosion media are difficult to contact with metal, so that the purpose of corrosion resistance is achieved; the impact liquid drops are bounced off before being frozen, and the freezing time of the liquid drops can be greatly delayed due to the low heat transfer efficiency of the attached liquid drops and the surface, so that the aim of preventing freezing is fulfilled; nano SiO2The particles are half embedded into the surface of the TPU coating, and the TPU coating has certain elasticity, so that external objects firstly touch the nano SiO2The particles can not directly act on the TPU coating, and in addition, the nano SiO2The particles have certain wear resistance, so the wear resistance of the coating is formed by nano SiO2The particles and the TPU coating act synergistically.
The invention adopts trimethoxy (1H,1H,2H, 2H-heptadecafluorodecyl) silane to nano SiO2The particles are subjected to hydrophobic modification to reduce the surface energy, and the concentration is low, the dosage is small, and the environmental pollution is small. The surface of the modified coating obtains excellent hydrophobicity, and has a contact angle of more than 150 degrees and a rolling angle of less than 10 degrees under acidic, neutral and weakly alkaline environments; preparation of the inventionThe anticorrosive anti-icing wear-resistant super-hydrophobic coating has excellent corrosion resistance, so that the corrosion current density is reduced by 3 orders of magnitude compared with that of a blank metal, the self-corrosion potential is obviously shifted forward, the impedance is increased by more than 300 times, the corrosion rate is effectively delayed, and the corrosion resistance is enhanced; the anticorrosive anti-icing wear-resistant super-hydrophobic coating prepared by the invention has better anti-icing capability, can effectively delay the icing time, and is nearly 3 times longer than that of a bare metal surface.
The anticorrosive anti-icing wear-resistant super-hydrophobic coating prepared by the invention simultaneously meets the anticorrosive anti-icing requirements of the surface of the metal substrate, reduces the safety risk of equipment and components, prolongs the service life, saves manpower, material resources and financial resources because only a common and conventional coating method is adopted, does not need special equipment, and can realize industrial production, thereby obtaining greater economic benefit.
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include such modifications and variations.

Claims (10)

1. The preparation method of the anticorrosive, anti-icing and wear-resistant super-hydrophobic coating is characterized by comprising the following steps of:
step 1, modifying nano SiO2Preparation of particles
Mixing nano SiO2The particles are immersed into a fluorosilane-absolute ethyl alcohol modified solution for modification at room temperature, and the modified nano SiO is2Drying the particles, and grinding and dispersing;
preparing a film forming solution: dissolving thermoplastic polyurethane elastomer rubber in N, N-dimethylformamide to prepare a film forming solution;
step 2, coating film
Coating the film forming liquid obtained in the step (1) on the surface of a pretreated base material by scraping, drying and cooling, and then repeatedly coating by scraping for many times to form a bottom film layer on the surface of the metal base material;
step 3, preparing the anticorrosive anti-icing wear-resistant super-hydrophobic coating
Coating the film forming solution prepared in the step 1 on the bottom film layer formed in the step 2 in a scraping manner to obtain a film coating layer; uniformly coating the modified nano SiO prepared in the step 1 on the surface of the coating layer2And (4) preparing a composite layer by using the particles, pressing the composite layer, and drying to obtain the anticorrosive anti-icing wear-resistant super-hydrophobic coating.
2. The preparation method of the anticorrosive, anti-icing and wear-resistant super-hydrophobic coating according to claim 1, wherein in step 1, the nano SiO is used before modification2The particle size of the particles is 10 to 20 nm.
3. The preparation method of the anticorrosive, anti-icing and wear-resistant super-hydrophobic coating according to claim 1, wherein in step 1, the nano SiO is2The modification time of the particles is 0.5-1 h, and the modified nano SiO2Drying the particles at 90-110 ℃ for 4-6 h.
4. The preparation method of the anticorrosive, anti-icing and wear-resistant super-hydrophobic coating according to claim 1, wherein in the step 1, the modified nano SiO is2The particle size of the particles is 20 to 40 nm.
5. The preparation method of the anticorrosive, anti-icing and wear-resistant super-hydrophobic coating according to claim 1, wherein the mass fraction of the fluorosilane in the fluorosilane-anhydrous ethanol modified solution is 0.8-1.5 wt%, and the nano SiO is2The mass ratio of the particles to the fluorosilane-absolute ethyl alcohol modified solution is 1: 20 to 25.
6. The preparation method of the anticorrosive, anti-icing and wear-resistant super-hydrophobic coating according to claim 1, wherein in the step 1, the concentration of the film forming solution is 0.3-0.35 g/ml; in the step 2, the repeated blade coating times are 3-5.
7. The preparation method of the anticorrosive, anti-icing and wear-resistant super-hydrophobic coating according to claim 1, wherein in the step 2, the thickness of the base film layer is 160-220 μm.
8. The preparation method of the anticorrosive, anti-icing and wear-resistant super-hydrophobic coating according to claim 1, wherein in the step 3, the pressing comprises the following specific steps: and placing the flat plate on the composite layer, and applying pressure of 10-50N to press for 5-10 min.
9. The preparation method of the corrosion-resistant, anti-icing and wear-resistant super-hydrophobic coating according to claim 1, wherein in the step 2, the pretreatment method of the substrate comprises the following steps: and (3) polishing the metal base material by using 80-400-mesh sand paper, cleaning the polished metal base material by using water and absolute ethyl alcohol successively, and airing for later use.
10. The anticorrosive anti-icing wear-resistant super-hydrophobic coating is prepared by the preparation method of any one of claims 1 to 9.
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113896430A (en) * 2021-10-28 2022-01-07 苏州大学 Adhesive composite wear-resistant super-hydrophobic coating and preparation method thereof
CN115109507A (en) * 2022-03-25 2022-09-27 国家能源集团宁夏煤业有限责任公司 Anticorrosive coating composition, anticorrosive coating, preparation method and application of anticorrosive coating, and anticorrosive coating
CN115466599A (en) * 2022-09-13 2022-12-13 中科融志国际科技(北京)有限公司 Transparent anti-icing coating and fan blade

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CN106893454A (en) * 2017-04-21 2017-06-27 黑龙江凯恩琪新材料科技有限公司 A kind of preparation method of sprayable and durable super-amphiphobic coating

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CN106893454A (en) * 2017-04-21 2017-06-27 黑龙江凯恩琪新材料科技有限公司 A kind of preparation method of sprayable and durable super-amphiphobic coating

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113896430A (en) * 2021-10-28 2022-01-07 苏州大学 Adhesive composite wear-resistant super-hydrophobic coating and preparation method thereof
CN115109507A (en) * 2022-03-25 2022-09-27 国家能源集团宁夏煤业有限责任公司 Anticorrosive coating composition, anticorrosive coating, preparation method and application of anticorrosive coating, and anticorrosive coating
CN115466599A (en) * 2022-09-13 2022-12-13 中科融志国际科技(北京)有限公司 Transparent anti-icing coating and fan blade
CN115466599B (en) * 2022-09-13 2024-03-12 中科融志国际科技(北京)有限公司 Transparent anti-icing coating and fan blade

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