CN115093790A - Preparation method of magnesium alloy surface super-hydrophobic anticorrosive coating - Google Patents
Preparation method of magnesium alloy surface super-hydrophobic anticorrosive coating Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
- C09D183/04—Polysiloxanes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D5/00—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
- B05D7/14—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials to metal, e.g. car bodies
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- 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
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- C—CHEMISTRY; METALLURGY
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- 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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- 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
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- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
Abstract
The invention provides a preparation method of a magnesium alloy surface super-hydrophobic anticorrosive coating, which comprises the steps of polishing a magnesium alloy step by step, cleaning, then drying in vacuum, uniformly spraying a super-hydrophobic coating liquid on the surface of the magnesium alloy subjected to vacuum drying, and continuously carrying out heat treatment to form the super-hydrophobic anticorrosive coating on the surface of the magnesium alloy; the super-hydrophobic micro-nano particles are prepared by the following method: ultrasonically dispersing the nano-fiber particles in a mixed solution of ethanol and ammonia water, dropwise adding silicate ester and a alkylating agent under continuous stirring, stirring for reaction at room temperature, centrifugally separating, and drying to obtain the hydrophobic micro-nano particles. The nano-fiber-silicon dioxide composite super-hydrophobic nano-particle is prepared by a sol-gel method, and the super-hydrophobic anti-corrosion coating with a bar-point micro/nano coarse structure on the surface of the magnesium alloy is prepared by bonding, spraying and thermosetting of a silane coupling agent. The obtained super-hydrophobic coating has obvious air cushion effect and good corrosion resistance.
Description
The invention relates to a divisional application of 'preparation methods of super-hydrophobic micro-nano particles with a bar dot structure, super-hydrophobic coating liquid and a super-hydrophobic anti-corrosion coating', wherein the application number of the divisional application is 2021103135566, and the application date is 2021, 03 and 24 days.
Technical Field
The invention relates to the technical field of metal corrosion prevention, in particular to super-hydrophobic micro-nano particles with a rod-point structure, super-hydrophobic coating liquid and a preparation method of a super-hydrophobic corrosion-resistant coating.
Background
The magnesium alloy has excellent physical and mechanical properties such as high strength/weight ratio, good castability, vibration reduction, high damping and the like, and is considered as an ideal material for light weight, fuel consumption reduction and carbon dioxide emission reduction of transportation tools. However, magnesium has low electrode potential, high chemical activity, loose oxide film, poor corrosion resistance of magnesium alloy, and is easily corroded particularly in aqueous solution or humid environment, which greatly limits the wide application of magnesium alloy.
The super-hydrophobic surface (the water contact angle is more than 150 degrees, and the sliding angle is less than 10 degrees) can effectively inhibit the contact of water and a metal matrix due to the excellent water repellency, and plays a role in protecting the chemical corrosion of the matrix. Chinese patent (CN103450801A) adopts a method of pyrolyzing silica gel and oxidizing vapor deposition under an aerobic atmosphere to prepare super-hydrophobic coatings on glass, battery pieces and metal. However, the method uses an oxygen atmosphere, which causes magnesium and magnesium alloy to form loose oxides, and the formed coating falls off, thus being not suitable for the coating preparation of magnesium and magnesium alloy. In Chinese patent (CN103305122B), an organic montmorillonite product of Nanocor company and fluorosilane modified silicon dioxide jointly form a super-hydrophobic surface under the action of a U.S. Dow Corning silicone rubber curing agent. Chinese patent (CN106189832B) alternately deposits organic polysilazane and fluorosilane modified inorganic nano-materials on the surface to obtain the super-hydrophobic coating. In the two technologies, due to the property of the coating material, a large amount of high-toxicity and explosive organic solvents such as tetrahydrofuran and the like are inevitably used in the mold making process, and the solvents volatilize in the thermosetting process, so that the pollution and the harm are caused to human bodies and the environment, and the potential safety hazard of combustion and explosion exists.
At present, a super-hydrophobic coating is prepared on the surface of a magnesium alloy, and the super-hydrophobic coating is prepared by roughening the surface of the magnesium alloy through methods such as micro-arc oxidation, chemical corrosion, electrodeposition and the like and then coating a hydrophobic substance. When the surface roughness is insufficient, the Cassie state is not stable enough, and the surface is easily transformed to the Wenzel wet state. Chinese patent (CN103088380A) takes an organic acid calcium nitrate ethanol solution as an electrolyte, and adopts an electrochemical deposition method to deposit calcium myristate on the surface of magnesium and magnesium alloy to prepare the super-hydrophobic coating. In the method, organic acid in the electrolyte and calcium ions generate precipitates under the action of an electric field on a cathode to form a super-hydrophobic coating, and the calcium myristate coating has certain water solubility and does not have strong acting force with magnesium and magnesium alloy, so that the formed coating is likely to fall off easily or be dissolved slowly in an aqueous solution. Chinese patent (CN101469425A) carries out micro-arc oxidation and annealing on the magnesium alloy, a rough structure is constructed on the surface of the magnesium alloy, and after the rough structure is treated by acrylic acid, the super-hydrophobic surface of the magnesium alloy is obtained by spin coating vinyl polydimethylsiloxane. The method needs special equipment for micro-arc oxidation and has limited preparation scale. Chinese patent (CN101824620A) adopts mixed solution of nitric acid and nitrate to carry out roughening treatment of chemical corrosion on the surface of the magnesium alloy, and then adopts silane hydrophobizing agent to soak the magnesium alloy to prepare the magnesium alloy surface super-hydrophobic coating. The method has simple process, but a large amount of acidic etching waste liquid is generated in acid soaking treatment, and subsequent acidic oxidizing waste liquid treatment equipment is required to be matched.
Disclosure of Invention
The invention aims to provide hydrophobic micro-nano particles with a rod point structure aiming at various defects existing in the preparation process of an anticorrosive coating on the surface of a magnesium alloy in the prior art.
It is another object of the present invention to provide a superhydrophobic coating solution based on the hydrophobic micro-nano particles.
The invention also aims to provide a preparation method of the super-hydrophobic anti-corrosion coating.
The technical scheme adopted for realizing the purpose of the invention is as follows:
a superhydrophobic micro-nanoparticle, the superhydrophobic micro-nanoparticle prepared by a method comprising: ultrasonically dispersing the nano-fiber particles in a mixed solution of ethanol and ammonia water, dropwise adding silicate ester and a alkylating agent under continuous stirring, stirring for reaction at room temperature, centrifugally separating, and drying to obtain the hydrophobic micro-nano particles.
In the above technical solution, the nanofiber particles are at least one of carbon nanofibers, glass nanofibers, attapulgite nanofibers, basic magnesium sulfate whiskers, basic magnesium chloride whiskers, magnesium oxide whiskers, aluminum oxide whiskers, magnesium borate whiskers, calcium carbonate whiskers, silicon carbide whiskers, silicon nitride whiskers, aluminum borate whiskers, or potassium titanate whiskers.
In the above technical solution, the hydrocarbylating agent is at least one of alkylsilane, hydrocarbyloxy chlorosilane, cycloaliphatic epoxy silane, and phenyl silane.
In the technical scheme, the volume ratio of the ethanol to the ammonia water is (1-10):1, the addition amount of the nanofiber particles is 10-200g/L, the addition amount of the silicate ester is 5-500mL/L, and the addition amount of the alkylating agent is 1-200 mL/L.
In another aspect of the present invention, the use of said superhydrophobic micro-nano particles in an anti-corrosive coating or a self-cleaning coating.
In another aspect of the present invention, a super-hydrophobic coating liquid is prepared by the following method:
In another aspect of the invention, the super-hydrophobic coating liquid is applied to an alloy as an anti-corrosion coating or applied to a fabric, glass or wood as a self-cleaning coating.
In the technical scheme, the silane coupling agent is at least one of methacryloxy silane, epoxy silane, vinyl silane, isocyanate silane and ureido silane; the silicate is at least one of methyl orthosilicate, ethyl orthosilicate, isopropyl orthosilicate and butyl orthosilicate. The rough structure of the coating is mainly contributed by the structures of coating rods and points, and the influence of the molecular chain length of the silane coupling agent in the binding liquid on the rough structure is small.
In the technical scheme, in the step 1, the volume ratio of ethanol to water is 80:1-10:1, the addition amount of the silane coupling agent is 20-400mL/L, the addition amount of silicate ester is 5-200mL/L, and the pH value of the system is 3.0-5.5.
In the technical scheme, in the step 2, the dosage of the super-hydrophobic micro-nano particles in the ethanol is 10-500g/L, and the addition amount of the coating binding liquid is 0.5-10L/L.
On the other hand, the invention provides a preparation method of the magnesium alloy surface super-hydrophobic anticorrosive coating, which comprises the steps of polishing the magnesium alloy step by step, cleaning, then drying in vacuum, uniformly spraying the super-hydrophobic coating liquid on the surface of the magnesium alloy dried in vacuum, and continuously carrying out heat treatment to form the super-hydrophobic anticorrosive coating on the surface of the magnesium alloy.
In the technical scheme, the vacuum drying temperature and the heat treatment temperature are both 70-150 ℃, and the heat treatment time is more than 10 min.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention provides a preparation method of a magnesium alloy surface super-hydrophobic anti-corrosion coating, which comprises the steps of preparing nanofiber-silicon dioxide composite super-hydrophobic nano particles through a sol-gel method, and preparing the super-hydrophobic anti-corrosion coating with a bar-point micro/nano coarse structure on the surface of a magnesium alloy through bonding, spraying and thermosetting of a silane coupling agent.
2. The obtained super-hydrophobic coating has obvious air cushion effect, good corrosion resistance, nontoxic and mild preparation conditions, avoids expensive fluorine-containing raw materials, has low preparation cost, simple and quick process and is easy for large-scale application.
Drawings
FIG. 1 SEM images of nano-fiber particles (a), hydrophobic micro-nano particles (b) and magnesium alloy surface super-hydrophobic anticorrosion coating (c).
FIG. 2 is a photo of the "air cushion effect" of the super-hydrophobic anticorrosion coating on the surface of the magnesium alloy.
FIG. 3 shows the contact angle and the rolling angle of the super-hydrophobic anticorrosion coating on the surface of the magnesium alloy.
FIG. 4 is a polarization plot of a blank sample and a superhydrophobic corrosion protection coating.
Detailed Description
The present invention will be described in further detail with reference to specific examples. It should be understood that the specific embodiments described herein are merely illustrative of the invention and do not limit the invention.
Example 1
1.1
A hydrophobic micro-nanoparticle, which is prepared by the following method: ultrasonically dispersing 5g of nano glass fiber particles in 500mL of mixed solution of 1:1 ethanol and ammonia water, dropwise adding tetramethyl orthosilicate and cyclohexyl trimethoxy silane under continuous stirring, stirring at room temperature for reacting for 6h, centrifugally separating, and drying at 80 ℃ to obtain the hydrophobic micro-nano particles.
1.2
A super-hydrophobic coating liquid is prepared by the following method:
1.3
A preparation method of a magnesium alloy surface super-hydrophobic anticorrosive coating comprises the following steps:
polishing the magnesium alloy to 1200#, cleaning with ethanol, vacuum drying at 70 ℃, uniformly spraying the super-hydrophobic coating liquid prepared in the embodiment 1.2 on the surface of the magnesium alloy preheated in vacuum at 70 ℃, and continuously carrying out heat treatment at 70 ℃ for 1h to form the super-hydrophobic anticorrosive coating on the surface of the magnesium alloy.
The contact angle of the coating is 157 degrees, the rolling angle is 5 degrees, and the corrosion current density is 7.691 multiplied by 10 -8 。
FIG. 1 is SEM images of nano-fiber particles (a), hydrophobic micro-nano particles (b) and a magnesium alloy surface super-hydrophobic anticorrosion coating (c), which can be seen from the images, on the surface of the magnesium alloy, the silicon dioxide nano particles in the hydrophobic micro-nano particles (b) are in a punctiform structure, the fiber whiskers are in a rod-shaped structure, the hydrophobic micro-nano particles (b) have an obvious rod-point micro/nano coarse structure, the alkylating agent has good hydrophobic property, and the fiber whisker and the silicon dioxide nano particle are combined together by covalent bonds as a modifier, so that the stability of the hydrophobic micro-nano particle (b) is improved, the hydrocarbylating agent used in the process does not contain fluorine, the cost is reduced, the process is green and environment-friendly, and a bar-point micro/nano rough structure is uniformly formed on the surface of the magnesium alloy as can be seen from an SEM image of the magnesium alloy surface super-hydrophobic anti-corrosion coating (c).
Fig. 2 is a photo of the air cushion effect of the super-hydrophobic anti-corrosion coating on the surface of the magnesium alloy, and it can be seen from the figure that the part immersed in water has an obvious silver mirror effect, which shows that the surface of the super-hydrophobic anti-corrosion coating has rich concave-convex rough structures, and forms rich micro bubbles by capturing air, so as to have the air cushion effect, and can well isolate the liquid phase, avoid corrosion contact, and thus play a good role in corrosion protection.
FIG. 3 shows the contact angle and the rolling angle of the super-hydrophobic anticorrosive coating on the surface of the magnesium alloy. The contact angle and the rolling angle of the coating are 157 degrees and 5 degrees, which shows that the super-hydrophobic coating with excellent performance is formed on the surface of the magnesium alloy.
Fig. 4 is a polarization plot of a blank sample and a superhydrophobic corrosion protection coating. It can be seen from the figure that the magnesium alloy with the super-hydrophobic anti-corrosion coating has obviously reduced corrosion current and greatly improved anti-corrosion performance compared with the magnesium alloy without the coating.
1.4
The super-hydrophobic coating liquid described in embodiment 1.2 can also be used as a self-cleaning material, and is sprayed on the surface of glass, wood or fabric, so that the self-cleaning function is achieved through the super-hydrophobic function.
Example 2
2.1
A hydrophobic micro-nanoparticle prepared by the following method: ultrasonically dispersing 20g of nano attapulgite fiber particles in 500mL of mixed solution of 5:1 ethanol and ammonia water, dropwise adding tetraethyl orthosilicate and diphenyl diethoxysilane under continuous stirring, stirring at room temperature for reacting for 8 hours, centrifugally separating, and drying at 100 ℃ to obtain the hydrophobic micro-nano particles.
2.2
A super-hydrophobic coating liquid is prepared by the following method:
2.3
A preparation method of a magnesium alloy surface super-hydrophobic anticorrosive coating comprises the following steps:
polishing the magnesium alloy to 1000# step by step, cleaning the magnesium alloy with ethanol, and drying the magnesium alloy in vacuum at 100 ℃; the super-hydrophobic coating liquid prepared in the example 2.2 is uniformly sprayed on the surface of the magnesium alloy preheated in vacuum at 100 ℃, and after heat treatment is carried out for 1h at 100 ℃, a super-hydrophobic anti-corrosion coating is formed on the surface of the magnesium alloy, wherein the contact angle of the coating is 159 degrees, the rolling angle is 4 degrees, and the corrosion current density is 5.519 multiplied by 10 -8 。
Example 3
3.1
A hydrophobic micro-nanoparticle, which is prepared by the following method: ultrasonically dispersing 20g of magnesium borate whisker particles in 500mL of a mixed solution of 5:1 ethanol and ammonia water, dropwise adding isopropyl n-silicate and 3-glycidyl ether oxypropyl triethoxysilane while continuously stirring, stirring at room temperature for reacting for 8 hours, centrifugally separating, and drying at 100 ℃ to obtain the hydrophobic micro-nano particles.
3.2
A super-hydrophobic coating liquid is prepared by the following method:
3.3
A preparation method of a magnesium alloy surface super-hydrophobic anticorrosive coating comprises the following steps: gradually polishing the magnesium alloy to 1200#, cleaning with ethanol, and vacuum drying at 80 ℃; the super-hydrophobic coating liquid prepared in the example 3.2 is uniformly sprayed on the surface of the magnesium alloy preheated in vacuum at the temperature of 80 ℃, and after the heat treatment is continuously carried out at the temperature of 150 ℃ for 0.5h, a super-hydrophobic anti-corrosion coating is formed on the surface of the magnesium alloy, wherein the contact angle, the rolling angle and the corrosion current density of the coating are respectively 160 degrees, 4 degrees and 2.044 degrees10 -10 。
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (5)
1. A preparation method of a magnesium alloy surface super-hydrophobic anticorrosive coating is characterized in that a magnesium alloy is polished step by step, cleaned and dried in vacuum, super-hydrophobic coating liquid is uniformly sprayed on the surface of the magnesium alloy which is dried in vacuum, and after continuous heat treatment, the magnesium alloy surface forms the super-hydrophobic anticorrosive coating;
wherein the super-hydrophobic coating liquid is prepared by the following method:
step 1, preparing a coating adhesive liquid: adding a silane coupling agent and silicate ester into an ethanol water solution, and adding acid to adjust the pH of the system under continuous stirring to obtain a bonding liquid of the coating; the silane coupling agent is at least one of methacryloxy silane, epoxy silane, vinyl silane, isocyanate silane and ureido silane, the silicate is at least one of methyl orthosilicate, ethyl orthosilicate, isopropyl orthosilicate and butyl orthosilicate, and the acid is citric acid or itaconic acid;
step 2, preparing super-hydrophobic coating liquid: dispersing the super-hydrophobic micro-nano particles in ethanol, and adding the coating adhesive liquid under continuous stirring to form uniform super-hydrophobic coating liquid; the super-hydrophobic micro-nano particles are prepared by the following method: ultrasonically dispersing nano-fiber particles in a mixed solution of ethanol and ammonia water, dropwise adding silicate ester and a alkylating agent under continuous stirring, stirring for reaction at room temperature, centrifugally separating, and drying to obtain super-hydrophobic micro-nano particles;
the hydrocarbylating agent is at least one of alkyl silane, alkoxy chlorosilane, alicyclic epoxy silane and phenyl silane.
2. The method according to claim 1, wherein the vacuum drying temperature and the heat treatment temperature are both 70 to 150 ℃ and the heat treatment time is more than 10 min.
3. The method of claim 1, wherein the nanofiber particles are at least one of carbon nanofibers, glass nanofibers, attapulgite fibers, magnesium oxysulfate whiskers, magnesium oxychloride whiskers, alumina whiskers, magnesium borate whiskers, calcium carbonate whiskers, silicon carbide whiskers, silicon nitride whiskers, aluminum borate whiskers, or potassium titanate whiskers.
4. The method according to claim 1, wherein the volume ratio of ethanol to ammonia water is 1-10:1, the amount of the nanofiber particles is 10-200g/L, the amount of the silicate is 5-500mL/L, and the amount of the hydrocarbylating agent is 1-200 mL/L.
5. The preparation method according to claim 1, wherein in the step 1, the volume ratio of ethanol to water is 80:1 to 10:1, the addition amount of the silane coupling agent is 20 to 400mL/L, the addition amount of the silicate is 5 to 200mL/L, and the pH of the system is 3.0 to 5.5;
in the step 2, the dosage of the super-hydrophobic micro-nano particles in the ethanol is 10-500g/L, and the addition amount of the coating binding liquid is 0.5-10L/L.
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| CN112724782B (en) * | 2020-12-28 | 2022-03-04 | 东北大学 | Preparation method of anti-corrosion self-healing super-hydrophobic material based on reversible hydrogen bond group |
| CN113462120A (en) * | 2021-08-20 | 2021-10-01 | 深圳市鑫俊通科技有限公司 | Self-cleaning silica gel keyboard key and preparation method thereof |
| CN116410629B (en) * | 2022-01-05 | 2024-02-27 | 中国科学院青海盐湖研究所 | Super-hydrophobic powder material and preparation method and application thereof |
| CN114436555A (en) * | 2022-01-21 | 2022-05-06 | 济南大学 | Modification method of calcium carbonate whisker, obtained product and application |
| CN115960530A (en) * | 2023-01-16 | 2023-04-14 | 陕西龙麟纳纤材料科技有限公司 | Calcium sulfate whisker composite silicon dioxide super-hydrophobic coating material and preparation method and application thereof |
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| CN113072877B (en) | 2022-08-23 |
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