CN108752987B - A kind of preparation method and applications of graphene-oxide composite coating - Google Patents
A kind of preparation method and applications of graphene-oxide composite coating Download PDFInfo
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- CN108752987B CN108752987B CN201810532453.7A CN201810532453A CN108752987B CN 108752987 B CN108752987 B CN 108752987B CN 201810532453 A CN201810532453 A CN 201810532453A CN 108752987 B CN108752987 B CN 108752987B
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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
- C09D1/00—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances
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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
- 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
- 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
Abstract
The present invention provides a kind of preparation method of graphene-metal oxide composite coating, first prepares the coating for including at least positive four butyl ester of 5wt%~10wt% metatitanic acid, 0.05wt%~1wt% Graphene derivative, 0.05wt%~1wt% surfactant, water and ethyl alcohol；Again by coating to spray, dip-coating, at least one of brushing method is in substrate material surface prepares coating；Film forming further is dried at a temperature of 100~400 DEG C in the coating of substrate material surface.Graphene of the invention-metal oxide composite coating its with excellent anticorrosive property, strong substrate caking power, and technique is controllable, can be applied to the surface covering protection of marine settings, new-energy automobile, building alloy material etc..
Description
Technical field
The invention belongs to the preparation fields of coating, further relate to a kind of technology of preparing of graphene-based composite coating.
Background technique
The high speed development of the development of the national economy, dependent on various metal materials building, machinery, ship, in terms of
Extensive use.However, metal erosion seriously affects the service life of various metal materials, and safety in production, life are brought
Huge hidden danger.The effective protection for realizing metal erosion is a global problem.Titanium dioxide is a kind of chemical, physical property
Extremely stable oxide, material acid-alkali-corrosive-resisting itself, simultaneously because it is cheap, based on titanium dioxide or add
The novel inorganic erosion shield of titanium dioxide is the hot spot of research and development；In addition, compared to the silica received significant attention
The alkaline resistance properties of coating, titanium dioxide is more excellent.However, single coating of titanium dioxide, compactness is poor, in practical application
In often Corrosion Protection it is bad.
Graphene is a kind of novel special material, and with ultra-thin and ultra-light, hard, surface modificability is strong, highly corrosion resistant
Property, high-wearing feature the advantages that, especially in terms of anticorrosion have good characteristic.The present invention utilizes the advantages of graphene, to change
The deficiency of kind titanium dioxide erosion shield, provides a kind of excellent graphene of Corrosion Protection-metal oxide composite coating,
The corrosion protection of all kinds of metal bases (including aluminium alloy, titanium alloy, kirsite and carbon steel etc.), application surface includes but is not limited to build
Build the surface covering of object structural material, the manufacture of ship yacht, marine monitoring equipment, new-energy automobile, space flight and aviation carrier etc.
Protection, sufficiently meets the market demand, has important application value.
Summary of the invention
It is an object of the present invention to which in view of the deficienciess of the prior art, to provide a kind of graphene-metal oxide compound
Coating.
Graphene of the present invention-metal oxide composite coating preparation method, successively comprises the steps of:
(A) prepare include at least positive four butyl ester of 5wt%~10wt% metatitanic acid, 0.05wt%~1wt% Graphene derivative,
The graphene of 0.05wt%~1wt% surfactant, water and ethyl alcohol-metal oxide composite coating；
(B) by graphene-metal oxide composite coating to spray, dip-coating, at least one of brushing method is in matrix
Material surface prepares coating；
(C) coating of substrate material surface is dried at a temperature of 100~400 DEG C, prepares graphene-metal oxidation
Object composite coating；
Graphene derivative in coating of the present invention is graphene oxide, graphene oxide ball, graphene oxide sheet, graphite
At least one of alkene, class graphene, graphene microchip, nano graphite flakes.The content of Graphene derivative be 0.05wt%~
1wt%, more excellent is 0.1wt%~0.5wt%.The particle diameter distribution D50 of Graphene derivative is 10 μm~30 μm, and more excellent is 20 μm
~30 μm.The median thickness of Graphene derivative is 2nm~10nm, and more excellent is 5nm~10nm.
Surfactant of the present invention is at least one of dodecyl sodium sulfate, alkyl phenol polyoxyethylene ether, and surface is living
Property agent content be 0.05wt%~1wt%, it is more excellent be 0.1wt%~0.5wt%.
The graphene-based coating of the present invention can be applied to any common in aluminium alloy, titanium alloy, kirsite and carbon steel
Metal matrix material.
The beneficial effects of the present invention are provide a kind of excellent anticorrosion, binding force strong metallic substrate surface protection
Coating.
Specific embodiment
It is an object of the present invention to which in view of the deficienciess of the prior art, to provide a kind of graphene-metal oxide compound
Coating.
Graphene of the present invention-metal oxide composite coating preparation method, successively comprises the steps of:
(D) prepare include at least positive four butyl ester of 5wt%~10wt% metatitanic acid, 0.05wt%~1wt% Graphene derivative,
The graphene of 0.05wt%~1wt% surfactant, water and ethyl alcohol-metal oxide composite coating；(E) by graphene-gold
Belong to oxide composite coating to spray, dip-coating, at least one of brushing method is in substrate material surface prepares coating；
(F) coating of substrate material surface is dried at a temperature of 100~400 DEG C, prepares graphene-metal oxidation
Object composite coating；
The particle diameter distribution D50 of Graphene derivative is 10 μm~30 μm in coating, and more excellent is 20 μm~30 μm, and graphene spreads out
The median thickness of biology is 2nm~10nm, and more excellent is 5nm~10nm.
Graphene derivative in coating of the present invention is graphene oxide, graphene oxide ball, graphene oxide sheet, graphite
At least one of alkene, class graphene, graphene microchip, nano graphite flakes, more excellent is graphene oxide sheet.Graphene derivative
Content it is more excellent be 0.1wt%~0.5wt%.
Surfactant of the present invention is at least one of dodecyl sodium sulfate, alkyl phenol polyoxyethylene ether, and surface is living
Property agent content it is more excellent be 0.1wt%~0.5wt%.
Further below by embodiment with the present invention will be described in detail.It will similarly be understood that following embodiment is served only for this
Invention is further described, and should not be understood as limiting the scope of the invention, those skilled in the art is according to this hair
Some nonessential modifications and adaptations that bright above content is made all belong to the scope of protection of the present invention.Following examples are specific
Technological parameter etc. is also only an example in OK range, i.e. those skilled in the art can be done properly by the explanation of this paper
In the range of select, and do not really want to be defined in hereafter exemplary specific value.
Embodiment 1
The preparation of graphene oxide: using graphite powder as raw material, preparing graphene oxide using improved Hummers method,
Natural graphite is predominantly aoxidized and passes through ultrasound removing by step can obtain finely dispersed graphene oxide colloidal suspensions,
Using the graphite powder of 8000 mesh, 200ml phosphoric acid, the 1800ml concentrated sulfuric acid, a small amount of repeatedly wheel are added first in the there-necked flask of ice bath
15g graphite powder, 90g potassium permanganate is added in stream, and 50 DEG C of reaction 12h after being cooled to room temperature, are added made of 3000ml deionized water
Ice cube.Finally reactant is poured into reactor, the hydrogen peroxide solution that 60ml 30wt% is added, which is reacted to bubble-free again, to be generated；
Addition and 1000mL hydrochloric acid, are centrifuged repeatedly, are washed with deionized, until solution neutral；It disperses the resulting solid in ethyl alcohol,
10mg/ml graphene oxide solution is prepared.The particle diameter distribution D of prepared graphene oxide50It is 10 μm, median thickness is
2nm。
The preparation of TiO 2 sol: positive four butyl ester of metatitanic acid is added in 100g dehydrated alcohol, stirs 1h, is solution A；
It is 0 that 100g ethyl alcohol is mixed with 100g deionized water and uses salt acid for adjusting pH, is solution B；Solution B is slowly added dropwise while stirring
Enter in solution A, stirring 5min is further continued for after being added dropwise to complete, prepares TiO 2 sol.Wherein the content of positive four butyl ester of metatitanic acid is
5wt%.
Graphene-metal oxide composite coating preparation: by graphene oxide dispersion, dodecyl sodium sulfate surface
Activating agent is added in TiO 2 sol, stirs 1h, graphene-metal oxide composite coating is made.Stone is aoxidized in coating
The content of black alkene is 0.05wt%, and the content of dodecyl sodium sulfate is 0.05wt%.
The preparation of graphene-metal oxide composite coating: it after aluminum alloy surface is handled, is hung down with the rate of 1cm/min
It is straight to immerse in graphene-metal oxide composite coating, 5min is kept, to lift in the graphene-based coating of the rate of 1cm/min,
Room temperature dries 10mim, and dry 30min, prepares graphene-based coating in aluminum alloy surface at 100 DEG C.
Embodiment 2
The content of graphene oxide is 0.07wt%, dodecyl sulphur in graphene-based coating unlike the first embodiment
The content of sour sodium is 0.07wt%, the particle diameter distribution D of graphene oxide50It is 15 μm, median thickness 5nm.
Embodiment 3
The content of graphene oxide is 0.1wt%, dodecyl sodium sulfonate in graphene-based coating unlike the first embodiment
The content of sodium is 0.1wt%, the particle diameter distribution D of graphene oxide50It is 20 μm, median thickness 7nm.
Embodiment 4
The content of graphene oxide is 0.5wt%, dodecyl sodium sulfonate in graphene-based coating unlike the first embodiment
The content of sodium is 0.5wt%, the particle diameter distribution D of graphene oxide50It is 25 μm, median thickness 8nm.
Embodiment 5
The content of graphene oxide is 0.7wt%, dodecyl sodium sulfonate in graphene-based coating unlike the first embodiment
The content of sodium is 0.7wt%, the particle diameter distribution D of graphene oxide50It is 27 μm, median thickness 8nm.
Embodiment 6
The content of graphene oxide is 1wt%, dodecyl sodium sulfate in graphene-based coating unlike the first embodiment
Content be 1wt%, the particle diameter distribution D of graphene oxide50It is 30 μm, median thickness 10nm.
Embodiment 7
The preparation of graphene oxide: using graphite powder as raw material, preparing graphene oxide using improved Hummers method,
Natural graphite is predominantly aoxidized and passes through ultrasound removing by step can obtain finely dispersed graphene oxide colloidal suspensions,
Using the graphite powder of 8000 mesh, 200ml phosphoric acid, the 1800ml concentrated sulfuric acid, a small amount of repeatedly wheel are added first in the there-necked flask of ice bath
15g graphite powder, 90g potassium permanganate is added in stream, and 50 DEG C of reaction 6h after being cooled to room temperature, are added made of 3000ml deionized water
Ice cube.Finally reactant is poured into reactor, the hydrogen peroxide solution that 60ml 30wt% is added, which is reacted to bubble-free again, to be generated；
Addition and 1000mL hydrochloric acid, are centrifuged repeatedly, are washed with deionized, until solution neutral；It disperses the resulting solid in ethyl alcohol,
10mg/ml graphene oxide solution is prepared.The particle diameter distribution D50 of prepared graphene oxide is 25 μm, median thickness
For 8nm.
The preparation of TiO 2 sol: positive four butyl ester of metatitanic acid is added in 100g dehydrated alcohol, stirs 1h, is solution A；
It is 0 that 100g ethyl alcohol is mixed with 100g deionized water and uses salt acid for adjusting pH, is solution B；Solution B is slowly added dropwise while stirring
Enter in solution A, stirring 5min is further continued for after being added dropwise to complete, prepares TiO 2 sol.Wherein the content of positive four butyl ester of metatitanic acid is
10wt%.
Graphene-metal oxide composite coating preparation: graphene-metal oxide composite coating preparation: by oxygen
Graphite alkene dispersion liquid, alkyl phenol polyoxyethylene ether are added in TiO 2 sol, stir 1h, graphene-metal oxygen is made
Compound composite coating.The content of graphene oxide is 1wt% in coating, and the content of alkyl phenol polyoxyethylene ether is 1wt%.
The preparation of graphene-metal oxide composite coating: after carbon steel is surface-treated, graphene-based coating spraying is arrived
Carbon steel surface, room temperature dry 10min, and dry 30min, is repeated 2 times, prepares graphene-based coating on carbon steel surface at 150 DEG C.
Embodiment 8
As different from Example 7, the content of positive four butyl ester of metatitanic acid is in graphene-metal oxide composite coating
5wt%, graphene-metal oxide composite coating drying temperature are 200 DEG C.
Embodiment 9
As different from Example 7, the content of positive four butyl ester of metatitanic acid is in graphene-metal oxide composite coating
7wt%, graphene-metal oxide composite coating drying temperature are 300 DEG C.
Embodiment 10
As different from Example 7, the content of graphene oxide is in graphene-metal oxide composite coating
0.05wt%, the content of alkyl phenol polyoxyethylene ether are 0.05wt%, graphene-metal oxide composite coating drying temperature
It is 400 DEG C.
Comparative example 1:
The preparation of TiO 2 sol: positive four butyl ester of metatitanic acid is added in 100g dehydrated alcohol, stirs 1h, is solution A；
It is 0 that 100g ethyl alcohol is mixed with 100g deionized water and uses salt acid for adjusting pH, is solution B；Solution B is slowly added dropwise while stirring
Enter in solution A, stirring 5min is further continued for after being added dropwise to complete, prepares TiO 2 sol.Wherein the content of positive four butyl ester of metatitanic acid is
10wt%.
The preparation of coating of titanium dioxide: after carbon steel is surface-treated, it is molten that titanium dioxide is dipped vertically into the rate of 1cm/min
In glue, 5min is kept, to lift in the rate TiO 2 sol of 1cm/min, room temperature dries 10min, dry at 200 DEG C
30min prepares coating of titanium dioxide on carbon steel surface.
Performance test: the titanium dioxide of the graphene of Examples 1 to 10-metal oxide composite coating, comparative example 1 applies
Layer carries out neutral NaCl salt spray test according to national standard GBT10125-2012, evaluates its mass loss after 1000h；According to GB
10124-88 carries out the total immersion test of acetic acid sodium chloride solution, evaluates mass loss rate after 500h；According to GBT12967.2-2008 into
The wearability of the graphene-based coating of row, coating is completely qualified after 1kg load, 20000 are enclosed, and it is unqualified for leaking out basis material；
According to the adhesive force of GB/T9286-1998 testing coating, 1mm spacing evaluates (0 grade: cut edge of rank after 10N/25mm test
Complete and smooth, nothing fall off).
As can be seen from the above table, the resistance to neutral salt spray of the graphene of Examples 1 to 10-metal oxide composite coating
The performances such as energy, the sodium chloride of resistance to acetic acid immersion corrosion performance, wearability are better than the coating of titanium dioxide of comparative example 1, and the above is only
It is all according to equivalent changes and modifications within the scope of the patent application of the present invention for presently preferred embodiments of the present invention, it should all belong to the present invention
Covering scope.
Claims (4)
1. a kind of graphene-metal oxide composite coating preparation method, it is characterised in that successively comprise the steps of:
(A) graphite powder for using 8000 mesh, the addition 200ml phosphoric acid first in the there-necked flask of ice bath, the 1800ml concentrated sulfuric acid, on a small quantity
15g graphite powder, 90g potassium permanganate is repeatedly added altogether in turn, after being cooled to room temperature, 3000ml deionization is added in 50 DEG C of reaction 12h
Ice cube made of water；Finally reactant is poured into reactor, the hydrogen peroxide solution that 60ml 30wt% is added is reacted to again without gas
Bubble generates；1000ml hydrochloric acid is added, is centrifuged repeatedly, is washed with deionized, until solution neutral；Disperse the resulting solid in second
In alcohol, 10mg/ml graphene oxide solution is prepared；The particle diameter distribution D of graphene oxide50It is 10 μm ~ 30 μm, intermediate value is thick
Degree is the nm of 2 nm ~ 10；
(B) positive four butyl ester of metatitanic acid is added in 100g dehydrated alcohol, stirs 1h, be solution A；By 100g ethyl alcohol and 100g go from
It is 0 that sub- water, which mixes and uses salt acid for adjusting pH, is solution B；Solution B is slowly added dropwise in solution A while stirring, after being added dropwise to complete
It is further continued for stirring 5min, prepares TiO 2 sol, wherein the content of positive four butyl ester of metatitanic acid is 5wt% ~ 10wt%；
(C) graphene oxide solution, surfactant are added in TiO 2 sol, stir 1h, graphene-metal is made
Oxide composite coating；The surfactant is at least one of dodecyl sodium sulfate, alkyl phenol polyoxyethylene ether；Table
The content of face activating agent is 0.05wt% ~ 1wt%；The content of graphene oxide is 0.05 ~ 1 wt% in coating；
(D) by after aluminium alloy or carbon steel surface treatment, it is compound that graphene-metal oxide is dipped vertically into the rate of 1cm/min
In coating, 5min is kept, to lift in the graphene-based coating of the rate of 1cm/min, room temperature dries 10mim, dry at 100 DEG C
30min prepares graphene-based coating in aluminium alloy or carbon steel surface.
2. a kind of preparation method of graphene-metal oxide composite coating as described in claim 1, it is characterised in that step
(C) content of surfactant is 0.1wt% ~ 0.7wt% in graphene-metal oxide composite coating.
3. a kind of preparation method of graphene-metal oxide composite coating as described in claim 1, it is characterised in that step
(C) content of graphene oxide is 0.1 ~ 0.5 wt% in graphene-metal oxide composite coating.
4. a kind of preparation method of graphene-metal oxide composite coating as described in claim 1, it is characterised in that step
(A) the particle diameter distribution D of the graphene oxide in50It is 15 μm ~ 25 μm, median thickness 5-8nm.
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| CN110157225B (en) * | 2019-04-15 | 2022-01-28 | 太原理工大学 | Preparation method of graphene-antibacterial antifouling anticorrosion composite coating on metal surface |
| CN113388315A (en) * | 2021-04-25 | 2021-09-14 | 中国科学院福建物质结构研究所 | Graphene/resin composite coating and preparation method of graphene/resin composite coating |
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