CN111574857B - Graphene-based nano composite anticorrosive paint and preparation method thereof - Google Patents

Graphene-based nano composite anticorrosive paint and preparation method thereof Download PDF

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CN111574857B
CN111574857B CN202010502790.9A CN202010502790A CN111574857B CN 111574857 B CN111574857 B CN 111574857B CN 202010502790 A CN202010502790 A CN 202010502790A CN 111574857 B CN111574857 B CN 111574857B
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acetone
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CN111574857A (en
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刘钰
帅世荣
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University of Electronic Science and Technology of China
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    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
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    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
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    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/12—Treatment with organosilicon compounds
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    • C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
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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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Abstract

The invention belongs to the technical field of epoxy coating anticorrosion, provides a graphene-based nano complex anticorrosion coating and a preparation method thereof, and aims to improve the dispersibility of a nano filler in epoxy resin. The method mainly comprises the following steps: firstly, gamma-aminopropyltriethoxysilane is used for modifying the surface of graphene oxide, and then the surface of graphene oxide is subjected to pi-pi stacking and phenyl silsesquioxane for modifying Fe3O4And compounding, namely adding the obtained phenyl silsesquioxane-graphene magnetic nano-composite dispersion liquid into epoxy resin and curing to obtain the phenyl silsesquioxane-graphene magnetic nano-composite based anticorrosive paint. The invention is a solvent-free type anticorrosive paint system, and the contained nano-composite can be stably and uniformly dispersed in the paint; meanwhile, an interpenetrating network structure is formed by crosslinking of the active groups reserved on the nano-composite and the epoxy resin, and the graphene is effectively prevented from being agglomerated in the using process. The invention improves the dispersibility of graphene in a polymer matrix.

Description

Graphene-based nano composite anticorrosive paint and preparation method thereof
Technical Field
The invention belongs to the technical field of epoxy coating anticorrosion, and particularly relates to a graphene-based nano composite anticorrosion coating and a preparation method thereof.
Background
Epoxy coatings have been widely used as corrosion resistant coatings for metal structures to resist corrosive substances such as oxygen, water, chloride ions, and the like. However, the micropores caused by the evaporation of the solvent during the curing of the epoxy resin become paths through which the electrolyte solution penetrates, so that the coating has poor corrosion resistance. To address this problem, nanofillers may be added to organic coatings to enhance their barrier properties and corrosion resistance. The nanofiller is capable of blocking micropores and cavities present in the coating matrix and reducing the diffusion of electrolyte to the coating/metal interface through tortuous electrolyte paths. In addition, the surface functionalization of the nano particles can increase the crosslinking density of the coating and further enhance the barrier property of the coating. In general, nanoparticles tend to agglomerate in epoxy resins, resulting in interfacial defects. Polyhedral oligomeric silsesquioxanes (POSS) have a synergistic effect of the compositional properties of organic and inorganic materials due to the nanostructured features of organic/inorganic hybrids, and can retain the original properties of modified epoxy resins to some extent. Therefore, the enhancement of the epoxy crosslinked network by the introduction of POSS is an effective means of modification. With POSS as a network crosslink, the polymer network can be reinforced by increasing crosslink density and blockiness of the rigid domains around the POSS units.
The presence of Graphene Oxide (GO) hydrophilic groups gives it excellent affinity for epoxy resins. The incorporation of GO into the epoxy matrix can enhance the mechanical properties, thermal stability and corrosion resistance of the epoxy resin, however, GO nanoplates have a tendency to self-polymerize in the polymer matrix due to high surface area and strong van der waals forces. To improve the interaction between the nanofiller interfaces in the polymer matrix, covalent and non-covalent modification of the GO nanoplates is required.
Therefore, the introduction of novel nanocomposites to improve nanofiller dispersibility in epoxy resins remains a challenge of current research value.
Disclosure of Invention
The invention provides a graphene-based nano-composite anticorrosive paint and a preparation method thereof, the prepared phenyl silsesquioxane-graphene magnetic nano-composite has good dispersibility in epoxy resin, can effectively improve crosslinking density and increase barrier property, thereby enhancing the anticorrosive property of the paint, and the composite paint has no solvent, is environment-friendly and is convenient to store, sell and use.
In order to achieve the purpose, the detailed process of the technical scheme of the invention comprises the following steps:
(1) introducing argon into a 500ml two-neck round-bottom flask for 10min, adding 12ml (0.05mol) phenyl triethoxy silicon, dropwise adding an acetic acid aqueous solution (0.1-5 wt%) by using a dropping funnel under an ice bath condition, reacting for 2-12h, placing the obtained transparent solution at-5-22 ℃ to obtain white precipitate, performing suction filtration and vacuum drying to obtain phenyl silanetriol;
(2) heating the phenyl silanetriol prepared in the step (1) and 3- (2, 3-epoxypropoxy) propyl trimethoxy silane (the mass fraction of the phenyl silanetriol is 20% -70%) in ethanol to 40-100 ℃, hydrolyzing for 1-6h, performing rotary evaporation to dryness, adding acetone to dissolve, performing rotary evaporation again to dryness, and performing vacuum drying to obtain phenyl silsesquioxane;
(3) the phenyl silsesquioxane prepared in the step (2) and the gamma-aminopropyltriethoxysilane modified Fe3O4(the weight percentage of the phenyl silsesquioxane is 10-90%) is heated to 40-100 ℃ in 100ml acetone and mechanically stirred for 2-24h, magnetically separated and washed with acetone for three times, and dried in vacuum to obtain Fe3O4@POSS；
(4) Using 10ml acetone as solvent, preparing Fe by the step (3)3O4@ POSS and gamma-aminopropyltriethoxysilane modified graphene oxide (Fe)3O4The mass fraction of @ POSS is 10% -90%), and then the mixture is subjected to ultrasonic treatment for 1-12h to obtain the phenyl silsesquioxane-graphene magnetic nano complex (Fe)3O4@POSS/GO）；
(5) Fe prepared in the step (4) is added3O4@ POSS/GO (with the mass fraction of 0.1wt% -2wt%) is added with a small amount of acetone for ultrasonic dispersion for 1-2h, and then added into 25g of epoxy resin, and mechanically stirred for dispersion for 20-30 min. Vacuumizing for 15-30min to remove acetone, taking out, adding a curing agent (the mass fraction is 10-35 wt%) under mechanical stirring, stirring for 5-15min, placing in a vacuum oven to remove bubbles, coating on a tin plate, and finally curing at 40-60 ℃ for 1-2h, 70-85 ℃ for 1-2h and 90-110 ℃ for 1-3 h;
preferably, the Fe3O4@ POSS/GO is 0.3wt% in the epoxy resin.
Preferably, the mass fraction of the curing agent D230 in the epoxy resin is 28 wt%.
The graphene-based nano complex anticorrosive paint preferably prepared by the invention is a solvent-free paint system, the paint fineness is less than 30 micrometers, and the water content of a paint film is less than 1%.
Compared with the prior art, the Fe prepared by the invention3O4The @ POSS/GO nano complex contains epoxy and amino active groups, can be used as a crosslinking point of epoxy resin to reinforce a crosslinking network and changeThe dispersibility of the nano filler is improved, and meanwhile, the composite is in a hydrophobic three-dimensional structure, so that the barrier property of the coating can be improved. The obtained anticorrosive paint based on the phenyl silsesquioxane-graphene magnetic nano complex does not contain an organic solvent, the fineness of the nano filler in the paint is 12 microns, the water content of a paint film after curing is lower than 1%, and the anticorrosive paint is convenient to spray and use, and is green and environment-friendly.
Drawings
FIG. 1 is a schematic representation of the preparation of a phenylsilsesquioxane of the present invention;
FIG. 2 shows Fe of the present invention3O4@ POSS preparation scheme;
FIG. 3 shows Fe of the present invention3O4The structure schematic diagram of @ POSS/GO;
FIG. 4 is a schematic view of the appearance of the composite coating and coating prepared according to the present invention;
FIG. 5 is a TGA profile of a composite coating paint film prepared according to example 2 of the present invention.
Detailed Description
The present invention will be further described with reference to the following specific examples.
Example 1
(1) Preparation of phenyl silsesquioxane
Argon is introduced into a 500ml two-neck round-bottom flask for 10min, 12ml (0.05mol) of phenyl triethoxy silicon is added, 5.4g of acetic acid aqueous solution (1.8 wt%) is dropwise added by a dropping funnel under an ice bath condition, then the reaction is carried out for 4h, the obtained transparent solution is refrigerated at 4 ℃, white precipitate appears after overnight, and phenyl silanetriol is obtained by vacuum filtration and drying. Heating 3- (2, 3-epoxypropoxy) propyl trimethoxy silane and phenyl silanetriol according to the molar ratio of 1:2 in ethanol to 80 ℃, hydrolyzing for 2h, carrying out rotary evaporation to dryness, adding acetone to dissolve, carrying out rotary evaporation again to dryness, and carrying out vacuum drying to obtain white solid phenyl silsesquioxane. The preparation process is shown in figure 1.
（2）Fe3O4Preparation of @ POSS
0.2g of phenyl silsesquioxane and 0.2g of gamma-aminopropyltriethoxysilane modified Fe are taken3O4Dissolving with 100ml acetone, reacting at 80 deg.C under the protection of argon gas with mechanical stirring for 12h, and magnetically separatingWashing with acetone for three times, and vacuum drying to obtain Fe3O4@ POSS. The preparation process is shown in figure 2.
（3）Fe3O4Preparation of @ POSS/GO
0.3g Fe in 10ml acetone solvent3O4Mixing @ POSS with 0.3g of gamma-aminopropyltriethoxysilane modified GO (graphene oxide colloid), and carrying out ultrasonic treatment for 6h to obtain Fe3O4@ POSS/GO, whose structure is shown in FIG. 3.
(4) Preparation of anticorrosive paint based on phenyl silsesquioxane-graphene magnetic nano complex
And (3) ultrasonically treating the tinplate with ethanol and acetone in sequence, and then drying the tinplate in an oven for later use. Subsequently, 0.025gFe3O4@ POSS/GO is added into 5ml of acetone for ultrasonic dispersion for 1 hour, then added into 25g of epoxy resin, and mechanically stirred and dispersed for 30 min. Vacuumizing for 15min to remove acetone, taking out, adding 7g of curing agent D230 under mechanical stirring, stirring for reacting for 5min, placing in a vacuum oven to remove bubbles, coating on a tin plate, and finally curing at 50 ℃ for 1h, at 80 ℃ for 2h and at 100 ℃ for 1 h. The composite coating and paint film are shown in FIG. 4.
Example 2
Example 2 was the same as example 1, except that Fe3O4@ POSS/GO is 0.075 g.
Example 3
Example 3 operates the same as example 1, the only difference being Fe3O4@ POSS/GO is 0.125 g.
The anti-corrosive paint films of graphene-based nanocomposite prepared in examples 1-3 were subjected to salt spray resistance evaluation, and the test was performed according to GB/T1771 for an experimental period of 10 days using a 5wt% aqueous solution of sodium chloride as a salt spray reagent. The results are shown in Table 1.
The moisture content of the composite coating paint film prepared in example 3 was measured by TGA as shown in figure 5. The loss of mass at 150 ℃ is due to the water content of the paint film itself, which means that the moisture content of the paint film is less than 1%, and the epoxy resin is decomposed into carbon dioxide and moisture at a temperature of 335 ℃ and 440 ℃ resulting in a rapid loss of paint film mass and finally a carbon chain skeleton remains.
It will be appreciated by those of ordinary skill in the art that the embodiments described herein are intended to assist the reader in understanding the principles of the invention and are to be construed as being without limitation to such specifically recited embodiments and examples. Those skilled in the art can make various other specific changes and combinations based on the teachings of the present invention without departing from the spirit of the invention, and these changes and combinations are within the scope of the invention.
Table-composite coating salt spray resistance evaluation
Sample (I) Resistance to salt spray (10)
Example 1 The paint film has smooth surface and rust lines only appear at the scratched part
Example 2 The paint film has smooth surface and rust lines only appear at the scratched part
Example 3 The paint film has smooth surface and rust lines only appear at the scratched part

Claims (10)

1. A preparation method of a graphene-based nanocomposite is characterized by comprising the following steps:
dropwise adding an acetic acid aqueous solution with the mass fraction of 0.1-5wt% into phenyl triethoxy silicon under the ice bath condition in the step (1), stirring for reacting for 2-12h, then placing at-5-22 ℃ to obtain white precipitate, performing suction filtration and vacuum drying to obtain phenyl silanetriol;
step (2) heating the phenyl silanetriol prepared in the step (1) and 3- (2, 3-epoxypropoxy) propyl trimethoxy silane in ethanol to 40-100 ℃, hydrolyzing for 1-6h, performing rotary evaporation to dryness, adding acetone to dissolve, performing rotary evaporation again to dryness, and performing vacuum drying to obtain phenyl silsesquioxane;
step (3) the phenyl silsesquioxane prepared in the step (2) is preparedFe modified by alkyl and gamma-aminopropyltriethoxysilane3O4Heating to 40-100 deg.C in acetone, mechanically stirring for 2-24h, magnetically separating, washing with acetone for three times, and vacuum drying to obtain Fe3O4@POSS；
Step (4) taking acetone as a solvent, and mixing the Fe prepared in the step (3)3O4Mixing the @ POSS and gamma-aminopropyltriethoxysilane modified graphene oxide, and performing ultrasonic treatment for 1-12h to obtain phenyl silsesquioxane-graphene magnetic nano complex Fe3O4@POSS/GO。
2. The method of claim 1, wherein the graphene-based nanocomposite comprises: the phenyl silsesquioxane is a double-epoxy double-layer cage-shaped silsesquioxane derivative.
3. The method of claim 1, wherein the graphene-based nanocomposite comprises: said Fe3O4@ POSS is Fe3O4The surface amino and the phenyl silsesquioxane epoxy group are in ring-opening coupling to form a three-dimensional structure.
4. The method of claim 1, wherein the graphene-based nanocomposite comprises: said Fe3O4The @ POSS/GO is the compound Fe of gamma-aminopropyltriethoxysilane-modified graphene oxide through pi-pi stacking effect3O4The spatial three-dimensional structure formed by the @ POSS.
5. The method of claim 1, wherein the graphene-based nanocomposite comprises: in the step (2), the mass fraction of the phenyl silanetriol is 20-70%.
6. The method of claim 1, wherein the graphene-based nanocomposite comprises: in the step (3), the mass fraction of the phenyl silsesquioxane is 10-90%.
7. The method of claim 1, wherein the graphene-based nanocomposite comprises: fe in step (4)3O4The mass fraction of @ POSS is 10-90%.
8. A graphene-based nanocomposite anticorrosive paint prepared by using the graphene-based nanocomposite according to any one of claims 1 to 7, wherein: fe prepared in the step (4) is added3O4Adding a small amount of acetone into the @ POSS/GO to perform ultrasonic dispersion for 1-2h, then adding the mixture into epoxy resin, and mechanically stirring and dispersing for 20-30 min; vacuumizing for 15-30min to remove acetone, and obtaining the anticorrosive paint.
9. The graphene-based nanocomposite anticorrosive paint according to claim 8, wherein: the anticorrosive paint is a solvent-free system, the fineness of the paint is less than 30 micrometers, and the moisture content of a paint film is less than 1%.
10. The graphene-based nanocomposite anticorrosive paint according to claim 8, wherein: said Fe3O4The @ POSS/GO nano composite accounts for 0.1-2% of the mass of the epoxy resin, and the curing agent accounts for 10-35%.
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