CN106752833A - A kind of preparation method of graphene oxide/silica composite coating - Google Patents
A kind of preparation method of graphene oxide/silica composite coating Download PDFInfo
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- CN106752833A CN106752833A CN201710038646.2A CN201710038646A CN106752833A CN 106752833 A CN106752833 A CN 106752833A CN 201710038646 A CN201710038646 A CN 201710038646A CN 106752833 A CN106752833 A CN 106752833A
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- graphene oxide
- composite coating
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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
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/04—Polyurethanes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/02—Ingredients treated with inorganic substances
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic 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
- C09D5/14—Paints containing biocides, e.g. fungicides, insecticides or pesticides
Abstract
The invention discloses a kind of preparation method of graphene oxide/silica composite coating, including prepare graphene oxide slurry;By graphene oxide slurry, cleaning to neutrality;After graphene oxide slurry is dried, it is distributed in water, ultrasound obtains graphene oxide uniform dispersion;Silica is added in obtained graphene oxide uniform dispersion, the step such as drying obtains solid product;Graphene oxide/silicon dioxide composite material is obtained;Above-mentioned composite is added into distilled water, ultrasonic disperse is carried out, graphene oxide/silicon dioxide composite material is configured to;Above-mentioned composite is mixed into addition distilled water with aqueous polyurethane, ultrasonic disperse is carried out, graphene oxide/silica composite coating is configured to.The preparation method of graphene oxide of the invention/silica composite coating, obtained composite coating while both having possessed stability high, good dispersion, has the functions such as formaldehyde adsorption, anion releasing, antibacterial bacteriostatic concurrently again.
Description
Technical field
The present invention relates to technical field of composite preparation, more particularly to a kind of graphene oxide/silica is combined
The preparation method of coating.
Background technology
Graphene oxide(GO)It is a kind of important graphite derivative, with specific surface energy higher, good hydrophily
And mechanical performance, there is substantial amounts of hydrophilic functional group in simultaneous oxidation Graphene, can be separately dispersed in water system and form oxidation
Graphene colloidal solution;Graphite oxide is that flake graphite is much larger than former graphite through a kind of interlamellar spacing that depth liquid phase oxidation is obtained
Lamellar compound, can form monolithic Rotating fields (i.e. graphene oxide) after stripping, be the important growth of Graphene, aoxidize stone
Black alkene has specific surface area big and the features such as ion-exchange capacity is strong.Through the graphite of peroxidating many has been introduced in its sheet surfaces
Oxy radical, such as hydroxyl, carboxyl, epoxy radicals hydrophilic active group, so that it is easy to form stabilization in polar solvent
Single sheet so that graphene oxide can be combined the composite wood for obtaining excellent performance with most metals and metal oxide
Material.
Silicon-dioxide powdery has excellent physicochemical property, includes crystal type and fusion, can be also divided into according to pattern
Spherical and angular, the species and particle diameter of the silica that different preparation methods is obtained differ widely, and silica is applied to
In coating new approach is opened to develop functional coating.How to select and be combined graphene oxide and other functional materials
To be that those skilled in the art have technical problem to be solved to the strong composite coating of feature.
The content of the invention
For defect present in prior art or deficiency, the present invention innovatively proposes a kind of graphene oxide/bis-
The preparation method of silica composite coating, makes obtained composite coating, while both having possessed stability high, good dispersion, and and
The functions such as tool formaldehyde adsorption, the pure and fresh, antibacterial bacteriostatic of anion.
The technical proposal of the invention is realized in this way:
A kind of preparation method of graphene oxide/silica composite coating, specifically includes following steps:
(1)Reacted with strong oxidizer with natural micron or nano-graphite, reaction temperature is 20-40 DEG C, and the reaction time is 1-3h, is obtained
To graphene oxide slurry;
(2)Take 1-2g steps(1)Obtained graphene oxide slurry, is cleaned to neutrality by the way of washing;
(3)By the drying of graphene oxide slurry, then the graphene oxide slurry after drying is distributed in water, ultrasound obtains oxygen
Graphite alkene uniform dispersion;
(4)Silica is added to step(3)In obtained graphene oxide uniform dispersion, stirring is ultrasonically treated, from
The heart, obtains graphene oxide-loaded SiO 2 powder solid product after drying;
(5)By step(4)Obtained solid product is added into deionized water, adds the mixing of hydrazine hydrate solution and concentrated ammonia liquor
Solution, is stirred, water-bath, and reaction is cooled down after terminating, and after washing, centrifugation, drying, obtains graphene oxide/dioxy
SiClx composite;
(6)To step(5)Obtained graphene oxide/silicon dioxide composite material adds distilled water, carries out ultrasonic disperse, ultrasound
Power is 60-180w, and ultrasonic time is set to 3-7h, is configured to graphene oxide/silicon dioxide composite material;
(7)By step(6)Obtained graphene oxide/silicon dioxide composite material is 1-10 with the mass ratio of aqueous polyurethane:
100 add distilled water, carry out ultrasonic disperse, and ultrasonic power is 60-180w, and ultrasonic time is set to 4-8h, are configured to aoxidize stone
Black alkene/silica composite coating.
Preferably, the step(5)Middle water-bath reaction temperature is 92-98 DEG C, and the water-bath time is 1.5-2.5h, described
The temperature of drying is 80-85 DEG C.
Preferably, the concentration of graphene oxide is 0.005%-1% in the uniform dispersion.
Preferably, the concentration of silica is 1.2%-6.5% in the uniform dispersion.
Preferably, the graphene oxide/silica composite coating and the mass ratio of aqueous polyurethane are 1-10:100.
Compared with prior art, the beneficial effects of the present invention are:
The invention discloses a kind of preparation method of graphene oxide/silica composite coating, make obtained composite coating, both
While possessing stability high, good dispersion, the work(such as pure and fresh formaldehyde adsorption, anion, antibacterial bacteriostatic, Low Temperature Far Infrared are had concurrently again
Energy.
In the preparation method, graphene oxide/silica be combined, Graphene have excellent Low Temperature Far Infrared, it is antibacterial,
The functions such as absorption, uvioresistant, silica has the functions such as excellent anion releasing, antibacterial bacteriostatic, uvioresistant.Oxidation stone
Black alkene is lyophobic dust, it is easy to reunited, and silica is combined with graphene oxide, can both improve the dispersion of graphene oxide
Property, at the same can play graphene oxide, the Low Temperature Far Infrared of silica, antibacterial bacteriostatic, absorption, uvioresistant and release bear from
The function of son.
Graphene oxide/silica the composite coating prepared using the preparation method, yield is high, it is easy to accomplish industrialization
Production.
Specific embodiment
With reference to specific embodiment, technical scheme is clearly and completely described, it is clear that retouched
The embodiment stated is only a part of embodiment of the invention, rather than whole embodiments.Based on the embodiment in the present invention, this
The every other embodiment that field those of ordinary skill is obtained under the premise of creative work is not made, belongs to the present invention
The scope of protection.
Embodiment 1:
A kind of preparation method of graphene oxide/silica composite coating, specifically includes following steps:
(1)The natural microns of 2g or nano-graphite are obtained into graphene oxide slurry with strong oxidizer potassium permanganate, nitric acid reaction, instead
Answer temperature for 20 DEG C, the reaction time is 1h;
(2)Take 1g steps(1)Obtained graphene oxide slurry, is cleaned to neutrality by the way of washing;
(3)Dried cleaning to neutral graphene oxide slurry, then the graphene oxide slurry after drying is distributed to 200ml
Water in, ultrasonic 20min obtains graphene oxide uniform dispersion;
(4)65g silica is added to step(3)In obtained graphene oxide uniform dispersion, stirring is ultrasonically treated to make
Silica is uniformly dispersed, and after ultrasonic 30min, centrifugation obtains graphene oxide-loaded SiO 2 powder after 70 DEG C of drying
Solid product;
(5)By step(4)Obtained solid product is added into deionized water, and the hydrazine hydrate for adding 30% percentage by volume is molten
The mixed solution of liquid and concentrated ammonia liquor, stirs, and mixing time is set to 10min, water-bath, and water-bath temperature is 92
DEG C, the water-bath time is 1.5h, and the temperature of the drying is 80 DEG C;Reaction terminate after cool down, through deionized water rinsing, from
After the heart, 70 DEG C of drying, graphene oxide/silicon dioxide composite material is obtained;
(6)To step(5)Obtained graphene oxide/silicon dioxide composite material adds distilled water, carries out ultrasonic disperse, ultrasound
Power is 60w, and ultrasonic time is set to 3h, is configured to graphene oxide/silicon dioxide composite material;
(7)By step(6)Obtained graphene oxide/silicon dioxide composite material is 5 with the mass ratio of aqueous polyurethane:100
Distilled water is added, ultrasonic disperse is carried out, ultrasonic power is 60w, and ultrasonic time is set to 5h, is configured to graphene oxide/dioxy
SiClx composite coating.
Embodiment 2:
A kind of preparation method of graphene oxide/silica composite coating, specifically includes following steps:
(1)The natural microns of 2g or nano-graphite are obtained into graphene oxide slurry with strong oxidizer potassium permanganate, nitric acid reaction, instead
Answer temperature for 30 DEG C, the reaction time is 2h;
(2)Take 1g steps(1)Obtained graphene oxide slurry, is cleaned to neutrality by the way of washing;
(3)Dried cleaning to neutral graphene oxide slurry, then the graphene oxide slurry after drying is distributed to 200ml
Water in, ultrasonic 35min obtains graphene oxide uniform dispersion;
(4)65g silica is added to step(3)In obtained graphene oxide uniform dispersion, stirring is ultrasonically treated to make
Silica is uniformly dispersed, and after ultrasonic 35min, centrifugation obtains graphene oxide-loaded SiO 2 powder after 70 DEG C of drying
Solid product;
(5)By step(4)Obtained solid product is added into deionized water, and the hydrazine hydrate for adding 30% percentage by volume is molten
The mixed solution of liquid and concentrated ammonia liquor, stirs, and mixing time is set to 10min, water-bath, and water-bath temperature is 95
DEG C, the water-bath time is 2h, and the temperature of the drying is 82 DEG C;Reaction terminate after cool down, through deionized water rinsing, centrifugation,
After 70 DEG C of drying, graphene oxide/silicon dioxide composite material is obtained;
(6)To step(5)Obtained graphene oxide/silicon dioxide composite material adds distilled water, carries out ultrasonic disperse, ultrasound
Power is 120w, and ultrasonic time is set to 5h, is configured to the multiple material of graphene oxide/silica;
(7)By step(6)Obtained graphene oxide/silicon dioxide composite material is 6 with the mass ratio of aqueous polyurethane:100
Distilled water is added, ultrasonic disperse is carried out, ultrasonic power is 120w, and ultrasonic time is set to 7h, is configured to graphene oxide/dioxy
SiClx composite coating.
Embodiment 3:
A kind of preparation method of graphene oxide/silica composite coating, specifically includes following steps:
(1), the natural microns of 2g or nano-graphite and strong oxidizer potassium permanganate, nitric acid reaction obtained into graphene oxide slurry,
Reaction temperature is 40 DEG C, and the reaction time is 3h;
(2), take 1g steps(1)Obtained graphene oxide slurry, is cleaned to neutrality by the way of washing;
(3), will clean to neutral graphene oxide slurry and dry, then the graphene oxide slurry after drying is distributed to
In the water of 200ml, ultrasonic 50min obtains graphene oxide uniform dispersion;
(4), 65g silica is added to step(3)In obtained graphene oxide uniform dispersion, stirring is ultrasonically treated
Silica is set to be uniformly dispersed, after ultrasonic 40min, centrifugation obtains graphene oxide-loaded silicon dioxide powder after 70 DEG C of drying
Last solid product;
(5), by step(4)Obtained solid product is added into deionized water, adds the hydrazine hydrate of 30% percentage by volume
The mixed solution of solution and concentrated ammonia liquor, stirs, and mixing time is set to 10min, water-bath, and water-bath temperature is 98
DEG C, the water-bath time is 2.5h, and the temperature of the drying is 85 DEG C;Reaction terminate after cool down, through deionized water rinsing, from
After the heart, 70 DEG C of drying, graphene oxide/silicon dioxide composite material is obtained;
(6), to step(5)Obtained graphene oxide/silicon dioxide composite material adds distilled water, carries out ultrasonic disperse, surpasses
Acoustical power is 180w, and ultrasonic time is set to 7h, is configured to graphene oxide/silica composite material;
(7)By step(6)Obtained graphene oxide/silicon dioxide composite material is 8 with the mass ratio of aqueous polyurethane:100
Distilled water is added, ultrasonic disperse is carried out, ultrasonic power is 180w, and ultrasonic time is set to 8h, is configured to graphene oxide/dioxy
SiClx composite coating.
The preferred embodiment of invention is the foregoing is only, is not intended to limit the invention, it is all in spirit of the invention
Within principle, any modification, equivalent substitution and improvements made etc. should be included within the scope of the present invention.
Claims (5)
1. the preparation method of a kind of graphene oxide/silica composite coating, it is characterised in that specifically include following steps:
(1)Reacted with strong oxidizer with natural micron or nano-graphite, reaction temperature is 20-40 DEG C, and the reaction time is 1-3h, is obtained
To graphene oxide slurry;
(2)Take 1-2g steps(1)Obtained graphene oxide slurry, is cleaned to neutrality by the way of washing;
(3)By the drying of graphene oxide slurry, then the graphene oxide slurry after drying is distributed in water, ultrasound obtains oxygen
Graphite alkene uniform dispersion;
(4)Silica is added to step(3)In obtained graphene oxide uniform dispersion, stirring is ultrasonically treated, from
The heart, obtains graphene oxide-loaded SiO 2 powder solid product after drying;
(5)By step(4)Obtained solid product is added into deionized water, adds the mixing of hydrazine hydrate solution and concentrated ammonia liquor
Solution, is stirred, water-bath, and reaction is cooled down after terminating, and after washing, centrifugation, drying, obtains graphene oxide/dioxy
SiClx composite;
(6)To step(5)Obtained graphene oxide/silicon dioxide composite material adds distilled water, carries out ultrasonic disperse, ultrasound
Power is 60-180w, and ultrasonic time is set to 3-7h, is configured to graphene oxide/silicon dioxide composite material;
(7)By step(6)Obtained graphene oxide/silicon dioxide composite material is 1-10 with the mass ratio of aqueous polyurethane:
100 add distilled water, carry out ultrasonic disperse, and ultrasonic power is 60-180w, and ultrasonic time is set to 4-8h, are configured to aoxidize stone
Black alkene/silica composite coating.
2. the preparation method of graphene oxide according to claim 1/silica composite coating, it is characterised in that institute
State step(5)Middle water-bath reaction temperature is 92-98 DEG C, and the water-bath time is 1.5-2.5h, and the temperature of the drying is 80-85
℃。
3. the preparation method of graphene oxide according to claim 1/silica composite coating, it is characterised in that institute
The concentration for stating graphene oxide in uniform dispersion is 0.005%-1%.
4. the preparation method of graphene oxide according to claim 1/silica composite coating, it is characterised in that institute
The concentration for stating silica in uniform dispersion is 1.2%-6.5%.
5. the preparation method of graphene oxide according to claim 1/silica composite coating, it is characterised in that institute
It is 1-10 that graphene oxide/silica composite coating is stated with the mass ratio of aqueous polyurethane:100.
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Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
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CN107353738A (en) * | 2017-07-20 | 2017-11-17 | 郑州氧乐环境科技有限公司 | A kind of water oxygen ecologic coating and preparation method thereof |
CN107540239A (en) * | 2017-10-26 | 2018-01-05 | 深圳大学 | Graphene oxide coats the preparation method of hollow glass microbead |
CN109504200A (en) * | 2018-10-11 | 2019-03-22 | 中国皮革制鞋研究院有限公司 | Composite paint and preparation method thereof |
CN111154392A (en) * | 2020-01-16 | 2020-05-15 | 河北工业大学 | Modified graphene oxide composite waterborne polyurethane environment-friendly anticorrosive paint |
CN112778892A (en) * | 2020-12-31 | 2021-05-11 | 重庆文理学院 | Method for preparing rod-shaped silicon dioxide-based composite photocatalytic antibacterial water-based interior wall paint |
CN112812669A (en) * | 2020-12-31 | 2021-05-18 | 重庆文理学院 | Method for preparing flower-like silicon dioxide-based composite photocatalytic antibacterial water-based interior wall paint |
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CN105131563A (en) * | 2015-09-30 | 2015-12-09 | 中北大学 | Preparation method for Fe3O4/graphene oxide/waterborne polyurethane composite |
CN105713519A (en) * | 2016-03-01 | 2016-06-29 | 山东农业大学 | Method for modifying water-borne wood coating by hybridizing two-dimensional graphene oxide and zero-dimensional inorganic nanoparticles |
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Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
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CN107353738A (en) * | 2017-07-20 | 2017-11-17 | 郑州氧乐环境科技有限公司 | A kind of water oxygen ecologic coating and preparation method thereof |
CN107540239A (en) * | 2017-10-26 | 2018-01-05 | 深圳大学 | Graphene oxide coats the preparation method of hollow glass microbead |
CN109504200A (en) * | 2018-10-11 | 2019-03-22 | 中国皮革制鞋研究院有限公司 | Composite paint and preparation method thereof |
CN111154392A (en) * | 2020-01-16 | 2020-05-15 | 河北工业大学 | Modified graphene oxide composite waterborne polyurethane environment-friendly anticorrosive paint |
CN111154392B (en) * | 2020-01-16 | 2022-01-11 | 河北工业大学 | Modified graphene oxide composite waterborne polyurethane environment-friendly anticorrosive paint |
CN112778892A (en) * | 2020-12-31 | 2021-05-11 | 重庆文理学院 | Method for preparing rod-shaped silicon dioxide-based composite photocatalytic antibacterial water-based interior wall paint |
CN112812669A (en) * | 2020-12-31 | 2021-05-18 | 重庆文理学院 | Method for preparing flower-like silicon dioxide-based composite photocatalytic antibacterial water-based interior wall paint |
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Application publication date: 20170531 |