CN108752987A - 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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- CN108752987A CN108752987A CN201810532453.7A CN201810532453A CN108752987A CN 108752987 A CN108752987 A CN 108752987A CN 201810532453 A CN201810532453 A CN 201810532453A CN 108752987 A CN108752987 A CN 108752987A
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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
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Abstract
The present invention provides a kind of preparation method of graphene-metal oxide composite coating, first prepares the coating including at least positive four butyl ester of 5wt%~10wt% metatitanic acids, 0.05wt%~1wt% Graphene derivatives, 0.05wt%~1wt% surfactants, 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-metal oxide composite coating of the present invention its with excellent anticorrosive property, strong substrate caking power, and technique is controllable, can be applied to the face coat 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 technology
The high speed development of the development of the national economy, dependent on various metal materials in building, machinery, ship, automobile etc.
Extensive use.However, metal erosion seriously affects the service life of various metal materials, and brought to keeping the safety in production, living
Huge hidden danger.Realize that the effective protection of 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 not limited to build
Build the face coat of object structural material, the manufacture of ship yacht, marine monitoring equipment, new-energy automobile, space flight and aviation carrier etc.
Protection, fully meets the market demand, has important application value.
Invention content
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.
The preparation method of graphene of the present invention-metal oxide composite coating, comprises the steps of successively：
(A) prepare including at least positive four butyl ester of 5wt%~10wt% metatitanic acids, 0.05wt%~1wt% Graphene derivatives,
The graphene of 0.05wt%~1wt% surfactants, 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 lived
Property agent content be 0.05wt%~1wt%, it is more excellent be 0.1wt%~0.5wt%.
It is common that the graphene-based coating of the present invention can be applied to any type 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 implementation mode
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.
The preparation method of graphene of the present invention-metal oxide composite coating, comprises the steps of successively：
(D) prepare including at least positive four butyl ester of 5wt%~10wt% metatitanic acids, 0.05wt%~1wt% Graphene derivatives,
The graphene of 0.05wt%~1wt% surfactants, 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 lived
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 the above 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 concrete numerical value.
Embodiment 1
The preparation of graphene oxide：Using graphite powder as raw material, graphene oxide is prepared using improved Hummers methods,
Natural graphite is predominantly aoxidized and passes through ultrasound stripping by step can obtain finely dispersed graphene oxide colloidal suspensions,
Using the graphite powder of 8000 mesh, 200ml phosphoric acid, the 1800ml concentrated sulfuric acids, a small amount of repeatedly wheel are added first in the there-necked flask of ice bath
15g graphite powders, 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 waters
Ice cube.Finally reactant is poured into reactor, the hydrogen peroxide solution that 60ml 30wt% are added is reacted to the generation of bubble-free again；
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 solutions are prepared.The particle diameter distribution D of prepared graphene oxide50It it is 10 μm, median thickness is
2nm。
The preparation of TiO 2 sol：Positive four butyl ester of metatitanic acid is added in 100g absolute ethyl alcohols, 1h is stirred, is solution A；
It is 0 that 100g ethyl alcohol is mixed with 100g deionized waters 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.The content of wherein positive four butyl ester of metatitanic acid is
5wt%.
The preparation of graphene-metal oxide composite coating：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：After aluminum alloy surface is handled, 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, graphene-based coating is prepared in aluminum alloy surface at 100 DEG C.
Embodiment 2
The content of graphene oxide is 0.07wt%, dodecyl sulphur in graphene-based coating as different from Example 1
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 as different from Example 1
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 as different from Example 1
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 as different from Example 1
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 as different from Example 1
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, graphene oxide is prepared using improved Hummers methods,
Natural graphite is predominantly aoxidized and passes through ultrasound stripping by step can obtain finely dispersed graphene oxide colloidal suspensions,
Using the graphite powder of 8000 mesh, 200ml phosphoric acid, the 1800ml concentrated sulfuric acids, a small amount of repeatedly wheel are added first in the there-necked flask of ice bath
15g graphite powders, 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 waters
Ice cube.Finally reactant is poured into reactor, the hydrogen peroxide solution that 60ml 30wt% are added is reacted to the generation of bubble-free again；
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 solutions are 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 absolute ethyl alcohols, 1h is stirred, is solution A；
It is 0 that 100g ethyl alcohol is mixed with 100g deionized waters 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.The content of wherein positive four butyl ester of metatitanic acid is
10wt%.
The preparation of graphene-metal oxide composite coating：The preparation of graphene-metal oxide composite coating：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, graphene-based coating is prepared 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
The drying temperature of 5wt%, graphene-metal oxide composite coating 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
The drying temperature of 7wt%, graphene-metal oxide composite coating are 300 DEG C.
Embodiment 10
As different from Example 7, the content of graphene oxide is in graphene-metal oxide composite coating
The content of 0.05wt%, alkyl phenol polyoxyethylene ether are 0.05wt%, the drying temperature of graphene-metal oxide composite coating
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 absolute ethyl alcohols, 1h is stirred, is solution A；
It is 0 that 100g ethyl alcohol is mixed with 100g deionized waters 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.The content of wherein 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 experiment according to national standard GBT10125-2012, its mass loss is evaluated after 1000h；According to GB
10124-88 carries out acetic acid sodium chloride solution total immersion test, and mass loss rate is evaluated after 500h；According to GBT12967.2-2008 into
The wearability of the graphene-based coating of row, coating is completely qualification after 1kg loads, 20000 are enclosed, and it is unqualified to leak out basis material；
According to the adhesive force of GB/T9286-1998 testing coatings, 1mm spacing evaluates (0 grade of rank after 10N/25mm tests：Cut edge
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
For presently preferred embodiments of the present invention, all equivalent changes and modifications done according to scope of the present invention patent should all belong to the present invention
Covering scope.
Claims (6)
1. a kind of preparation method of graphene-metal oxide composite coating, it is characterised in that comprise the steps of successively：
(A) prepare including at least positive four butyl ester of 5wt%~10wt% metatitanic acids, 0.05wt%~1wt% Graphene derivatives,
The graphene of 0.05wt%~1wt% surfactants, 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 basis material
Surface prepares coating；
(C) coating of substrate material surface is dried at a temperature of 100~400 DEG C, it is multiple prepares graphene-metal oxide
Close coating；
The particle diameter distribution D of Graphene derivative in the coating50It it is 10 μm~30 μm, the median thickness of Graphene derivative is
2nm~10nm；Surfactant is at least one of dodecyl sodium sulfate, alkyl phenol polyoxyethylene ether.
2. a kind of preparation method of graphene-metal oxide composite coating as described in claim 1, it is characterised in that step
(A) Graphene derivative in coating is graphene oxide, graphene oxide ball, graphene oxide sheet, graphene, class graphite
At least one of alkene, graphene microchip, nano graphite flakes.
3. a kind of preparation method of graphene-metal oxide composite coating as described in claim 1, it is characterised in that step
(A) content of surfactant is 0.1wt%~0.5wt% in 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) content of the Graphene derivative in coating is 0.1wt%~0.5wt%.
5. 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 derivative in coating50It is 20 μm~30 μm.
6. a kind of preparation method of graphene-metal oxide composite coating as described in claim 1, it is characterised in that step
(A) median thickness of the Graphene derivative in coating is 5nm~10nm.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109796137A (en) * | 2019-03-22 | 2019-05-24 | 江苏辉伦太阳能科技有限公司 | A kind of film plating process of photovoltaic self-cleaning glass |
| CN110157225A (en) * | 2019-04-15 | 2019-08-23 | 太原理工大学 | A kind of preparation method of metal surface graphene-antifouling corrosion-resistant composite coating of antibacterial |
| 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 |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105754383A (en) * | 2016-02-25 | 2016-07-13 | 中国科学院福建物质结构研究所 | Preparation method and application of graphene-based coating for marine device |
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- 2018-05-29 CN CN201810532453.7A patent/CN108752987B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105754383A (en) * | 2016-02-25 | 2016-07-13 | 中国科学院福建物质结构研究所 | Preparation method and application of graphene-based coating for marine device |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109796137A (en) * | 2019-03-22 | 2019-05-24 | 江苏辉伦太阳能科技有限公司 | A kind of film plating process of photovoltaic self-cleaning glass |
| CN110157225A (en) * | 2019-04-15 | 2019-08-23 | 太原理工大学 | A kind of preparation method of metal surface graphene-antifouling corrosion-resistant composite coating of antibacterial |
| 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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