CN112724782B - Preparation method of anti-corrosion self-healing super-hydrophobic material based on reversible hydrogen bond group - Google Patents
Preparation method of anti-corrosion self-healing super-hydrophobic material based on reversible hydrogen bond group Download PDFInfo
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Abstract
The invention discloses a preparation method of an anti-corrosion self-healing super-hydrophobic material based on reversible hydrogen bond groups, and particularly discloses a preparation method of a self-healing coating for rapidly repairing chemical damage at room temperature. The method comprises the following steps of coupling lignocellulose and ceramic nanoparticles with surfaces rich in hydroxyl with hydrolyzed octadecyl triethoxy silane self-healing agent through hydrogen bonds, preparing the super-hydrophobic anticorrosive coating by using epoxy resin and polyamide resin as adhesives, and further modifying a substrate coated on the surface of the material through octadecyl triethoxy silane to obtain an anticorrosive super-hydrophobic coating with a spontaneous healing function after chemical damage at room temperature; in addition, the pore material is dipped into the coating, and the coating has the oil-water separation function after the curing treatment. The self-healing super-hydrophobic coating prepared by the method has low cost, can realize the function of spontaneous healing after chemical damage occurs on the surface of a material, can be quickly recovered at room temperature without additional auxiliary action, and has anti-corrosion performance and wide application.
Description
Technical Field
The invention belongs to the technical field of self-healing super-hydrophobic materials, and relates to a preparation method of an anti-corrosion self-healing super-hydrophobic material based on reversible hydrogen bonds.
Background
With the discovery of self-healing materials, it is recognized that superhydrophobic coatings capable of healing physical or chemical damage have many potential applications, such as in the fields of self-cleaning, corrosion protection, ice and snow protection, oil-water separation, and the like. The self-healing super-hydrophobic coating mainly comprises a rough micro-nano structure and a low-surface-energy self-healing agent. The micro-nano structure can be prepared by various methods such as electrodeposition, corrosion, photoetching, templates, sol-gel and the like, and has complex process and high requirement on equipment; materials that can be used as self-healing agents are: low surface energy materials such as polydimethylsiloxane, octadecyltriethoxysilane, fluorosilane, etc. Self-healing agents, as a core part of repairing chemically damaged coatings, have been stored in micro-nanostructures by means of chemical bonds, electrostatic interactions and physical storage to date. However, coatings that employ chemical bonds coupled to self healing agents often require additional stimuli, such as temperature, light, humidity, etc., to activate the self healing capabilities of the coating; self-healing agent coatings coupled through electrostatic interaction are generally tedious in preparation process and relatively high in preparation cost; self-healing agents that employ physical storage are often susceptible to evaporation and/or degradation, reducing the coating's ability to be recycled. Until now, reports on hydrogen-bonding-based self-healing coatings have focused on the field of physical structural damage (e.g., cutting, scratching, etc.) of the healing coating, and self-healing techniques of coating surface chemistry and superhydrophobic capability have been left blank after chemical damage has occurred. The self-healing coating based on the reversible hydrogen bonds can be coupled with a large amount of self-healing agents and has a certain protection effect on the self-healing agents, and the self-healing capacity and the recycling stability of the coating are improved. Based on the characteristic that hydrogen bonds are easy to break and reform, after the surface of the material is chemically damaged, the hydrogen bond radical self-healing coating does not need additional stimulation, and rapid, efficient and spontaneous healing can be realized at room temperature.
Disclosure of Invention
The invention provides a preparation method of an anti-corrosion self-healing super-hydrophobic material based on reversible hydrogen bonds.
The technical scheme of the invention is as follows:
a preparation method of an anti-corrosion self-healing super-hydrophobic material based on reversible hydrogen bond groups comprises the following steps:
(1) mixing lignocellulose with hydroxyl on the surface and ceramic nanoparticles with hydroxyl on the surface with a hydrolyzed octadecyl triethoxy silane self-healing agent in a mass ratio of 0.1-1.2: 5-10: 1, reacting at room temperature for 2-24 hours, and separating and purifying with absolute ethyl alcohol to obtain modified super-hydrophobic micro-nano particles;
(2) mixing epoxy resin and polyamide resin with the modified super-hydrophobic micro-nano particles obtained in the step (1) according to a mass ratio of 1-4: 0.5-2: 1, adding ethanol, fully dissolving, stirring and performing ultrasonic treatment for 1-6 hours to prepare a uniform super-hydrophobic coating;
(3) coating the super-hydrophobic coating obtained in the step (2) on the surface of a base material, and then drying the base material in the air at room temperature; after drying, the anti-corrosion super-hydrophobic coating with rapid, efficient and spontaneous healing of chemical damage at room temperature is obtained.
Further, the anticorrosion super-hydrophobic coating obtained in the step (3) and the matrix are dipped in an ethanol solution containing 0.25-2.5 wt% of octadecyl triethoxy silane, then taken out, washed by ethanol, dried and cured. The purpose of the re-impregnation is to increase the content of the self-healing agent octadecyltriethoxysilane.
Preferably, the mass ratio of the lignocellulose with hydroxyl on the surface and the ceramic nano particles with hydroxyl on the surface to the hydrolyzed octadecyl triethoxy silane self-healing agent is 0.5-0.8: 5-8: 1.
Preferably, epoxy resin and polyamide resin are selected, and the mass ratio of the epoxy resin to the modified super-hydrophobic micro-nano particles obtained in the step (1) is 1-1.5: 0.5-1: 1.
Further, the particle size of the ceramic nano-particles is less than 100 nm.
Further, the particle size of the lignocellulose is 5-30 μm.
The base material in the step (3) comprises fiber fabric and metal aluminum.
The preparation method is simple and low in cost, and the self-healing anticorrosion super-hydrophobic coating based on the reversible hydrogen bond is prepared by controlling the reaction of the lignocellulose and ceramic nano particles and the hydrolyzed octadecyl triethoxy silane and the curing of the coating. The self-healing super-hydrophobic coating prepared can realize the function of spontaneous healing after chemical damage occurs to the surface of the material, can realize the quick recovery of the chemical composition and the super-hydrophobic property of the coating without additional auxiliary action at room temperature, has the anti-corrosion property, can be used for protective coatings of pipelines, outdoor buildings and the like, and has the oil-water separation function for pore materials of the impregnating coating.
Drawings
Fig. 1(a) is a scanning electron micrograph of a self-healing superhydrophobic coating based on reversible hydrogen bonds.
FIG. 1(b) is an infrared plot of the products produced by the different reaction steps.
FIG. 2(a) is a potentiodynamic polarization curve of a self-healing superhydrophobic coating;
fig. 2(b) is a relation between the self-healing time and the water contact angle of the self-healing super-hydrophobic coating after chemical damage.
FIG. 3(a) is a graph of self-healing time versus water contact angle after chemical damage for a superhydrophobic coating prepared by immersion in 0.25 wt% self-healing agent;
fig. 3(b) is a relation between the self-healing time and the water contact angle of the prepared covalent bond-based self-healing super-hydrophobic coating after chemical damage.
Fig. 4 is a relation between the oil-water separation efficiency and the separation times of the self-healing super-hydrophobic fiber fabric.
Detailed Description
The invention is described in detail below with reference to the figures and examples.
Example 1
Adding 10mL of ammonia water into a mixture containing 180mL of ethanol, 20mL of tetraethyl silicate and 20mL of deionized water, stirring for 12 hours at room temperature, and drying at 50 ℃ to obtain silicon dioxide nanoparticles with the particle size of 35 +/-5 nm; adding 1mL of octadecyltriethoxysilane into 70mL of ethanol containing 0.5g of lignocellulose and 6g of prepared silicon dioxide, respectively carrying out ultrasonic and stirring reaction on the suspension at 25 ℃ for 2 hours, washing and purifying the centrifuged particles by ethanol, and drying at room temperature to obtain super-hydrophobic micro/nano particles; adding 3g of super-hydrophobic powder into 80mL of ethanol solution containing 3g of epoxy resin and 2g of polyamide resin, and sequentially carrying out ultrasonic treatment and magnetic stirring for 2 hours respectively to finally obtain the uniform super-hydrophobic coating.
The super-hydrophobic coating is coated on the surface of the metal aluminum in a spraying way, and the spraying process comprises the following steps: spray coating for 30 seconds at a pressure of 1 atm. The coated aluminum substrate was then dried in air at room temperature for 2 hours. Finally, the coated aluminum substrate was further hydrophobically modified by immersing it in an ethanol solution containing 1.0 wt% of octadecyltriethoxysilane for 1 hour. And washing the prepared sample with ethanol to remove unreacted molecules, and then curing and drying at 25 ℃ for 24 hours to finally obtain the anti-corrosion self-healing super-hydrophobic coating with reversible hydrogen bond groups on the surface of the aluminum.
The reversible hydrogen bonds can store a large amount of self-healing agents and have a certain protection effect on the self-healing agents, and the original surface chemical composition and the super-hydrophobicity of the chemically damaged coating can be rapidly recovered at room temperature (4 hours).
Observing the self-healing super-hydrophobic coating prepared on the surface of the aluminum matrix under a scanning electron microscope, the prepared coating has a porous rough structure as shown in figure 1(a), and infrared curves of products prepared in different reaction steps are shown in figure 1 (b). Wherein the infrared curve of the silicon dioxide powder is 3448cm-1The peak is the stretching vibration peak of the hydroxyl group, and the red shift and broadening of the hydroxyl group peak to a low wave number indicate that hydrogen bonds exist in the product. Through testing, the prepared coating has excellent corrosion resistance, as shown in figure 2 (a). When the coating is chemically damaged, only 4 hours are required to restore the original superhydrophobic property at room temperature, as shown in fig. 2 (b).
Example 2
The difference from the embodiment 1 is that:
the coated aluminum substrate was further hydrophobically modified by immersing it in an ethanol solution containing 0.25 wt% of octadecyltriethoxysilane for 1 hour.
Through testing, the prepared coating has excellent self-healing performance, as shown in fig. 3 (a). When the coating is chemically damaged, only 10 hours are required to restore the original superhydrophobic property at room temperature. The superhydrophobic coating prepared under this condition still has a self-healing time much faster than that of the superhydrophobic coating prepared in the form of covalent bonds by curing at a high temperature of 100 ℃ for 2 hours, and as shown in fig. 3(b), the self-healing time of the covalently bonded superhydrophobic coating is about 24 hours at room temperature.
Example 3
The difference from the embodiment 1 is that:
and (3) coating the super-hydrophobic coating on the surface of the fiber fabric in a dipping mode, and curing to prepare the super-hydrophobic fiber fabric with self-healing capability. Wherein, the dipping process comprises the following steps: the fabric was completely immersed in the coating for 1 minute.
Tests prove that the prepared super-hydrophobic fiber fabric has excellent oil-water separation performance, and the oil-water separation capability is reduced after the super-hydrophobic fiber fabric is damaged by oil pollution; after ethanol washing, it took 4 hours to recover the original oil-water separation capacity at room temperature, as shown in fig. 4.
Claims (6)
1. A preparation method of an anti-corrosion self-healing super-hydrophobic material based on a reversible hydrogen bond group is characterized by comprising the following steps:
(1) mixing lignocellulose with hydroxyl on the surface and ceramic nanoparticles with hydroxyl on the surface with a hydrolyzed octadecyl triethoxy silane self-healing agent in a mass ratio of 0.1-1.2: 5-10: 1, reacting at room temperature for 2-24 hours, and separating and purifying with absolute ethyl alcohol to obtain modified super-hydrophobic micro-nano particles;
(2) mixing epoxy resin and polyamide resin with the modified super-hydrophobic micro-nano particles obtained in the step (1) according to a mass ratio of 1-4: 0.5-2: 1, adding ethanol, fully dissolving, stirring and performing ultrasonic treatment for 1-6 hours to prepare a uniform super-hydrophobic coating;
(3) coating the super-hydrophobic coating obtained in the step (2) on the surface of a base material, and then drying the base material in the air at room temperature; after drying, obtaining the anti-corrosion super-hydrophobic coating which has the advantages of rapidness, high efficiency and spontaneous healing of chemical damage at room temperature;
(4) and (3) dipping the anticorrosive super-hydrophobic coating obtained in the step (3) and the matrix in an ethanol solution containing 0.25-2.5 wt% of octadecyl triethoxy silane, taking out, cleaning with ethanol, drying and curing.
2. The preparation method of the anticorrosion self-healing super-hydrophobic material based on reversible hydrogen bonds is characterized in that the mass ratio of the lignocellulose with hydroxyl groups on the surface and the ceramic nanoparticles with hydroxyl groups on the surface to the hydrolyzed octadecyltriethoxysilane self-healing agent is 0.5-0.8: 5-8: 1.
3. The preparation method of the corrosion-proof self-healing super-hydrophobic material based on the reversible hydrogen bond is characterized in that the mass ratio of the epoxy resin to the polyamide resin to the modified super-hydrophobic micro-nano particles obtained in the step (1) is 1-1.5: 0.5-1: 1.
4. The preparation method of the anticorrosion self-healing super-hydrophobic material based on reversible hydrogen bonds as claimed in claim 1, wherein the ceramic nanoparticles have a particle size of less than 100 nm.
5. The preparation method of the corrosion-prevention self-healing super-hydrophobic material based on the reversible hydrogen bonding group according to claim 1, wherein the particle size of the lignocellulose is 5-30 μm.
6. The preparation method of the corrosion-prevention self-healing superhydrophobic material based on reversible hydrogen bonding group according to claim 1, wherein the matrix material in the step (3) comprises fiber fabric and metallic aluminum.
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CN102702553A (en) * | 2012-06-29 | 2012-10-03 | 山东轻工业学院 | Method for preparing inorganic particle/epoxy resin super hydrophobic film |
CN111019482A (en) * | 2019-12-24 | 2020-04-17 | 齐鲁工业大学 | Preparation and application of super-hydrophobic/oleophobic coating with excellent performance |
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