CN109096913A - A kind of preparation method and application of not fluorine-containing graphene-organic siliconresin super hydrophobic coating - Google Patents
A kind of preparation method and application of not fluorine-containing graphene-organic siliconresin super hydrophobic coating Download PDFInfo
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- CN109096913A CN109096913A CN201810661685.2A CN201810661685A CN109096913A CN 109096913 A CN109096913 A CN 109096913A CN 201810661685 A CN201810661685 A CN 201810661685A CN 109096913 A CN109096913 A CN 109096913A
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- graphene
- fluorine
- organic siliconresin
- hydrophobic 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
- C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
- C09D183/04—Polysiloxanes
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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
- C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
Abstract
The present invention relates to a kind of preparation method and applications of not fluorine-containing graphene-organic siliconresin super hydrophobic coating.Organic fluoride is used by limitation in the world since its superpower chemical stability causes to be difficult to decompose.The present invention combines graphene with organic siliconresin by physics mode and chemical mode, and the good super-hydrophobic coat of storage stability can be obtained by simple process.The resulting super-hydrophobic coat of the present invention has good mechanical performance and chemical stability, and static water droplet contact angle is greater than 150 °, has certain electric conductivity, has a extensive future in waterproof anti-ice, the heating that is powered, anti-electromagnetic shielding and antistatic field.
Description
Technical field
The invention belongs to super-hydrophobic coat technical fields, and in particular to a kind of not fluorine-containing graphene-organic siliconresin is super
The preparation method and application of hydrophobic coating.
Background technique
Super hydrophobic surface refers generally to water droplet and is in contact with it angle greater than 150 °, surface of the roll angle less than 10 °.It has from clear
The good characteristics such as clean, anti-adhesive, waterproof, so that super hydrophobic material is in waterproof clothes, exterior coating, electronic component, grease point
Very extensive application prospect is shown from fields such as, biological medicines.To ask hydrophobic effect, the preparation of existing super hydrophobic surface
Method is mostly to add the organic fluoride-containing compound of pole low-surface-energy.However due to carbon key fluoro- in organic fluoride-containing compound structure
Bond energy is extremely strong, so that the chemical property of this substance is extremely stable, can be subjected to high temperature, illumination, most chemical reactions, micro-
The metabolism of biological effect and animals and plants.Ecological environment problem and the human health danger that may cause in view of substance of this kind
Evil has had Countries and area to be included in some fluorinated organic compounds and be forbidden to use list.In addition, coating surface is received
Micro-structure is easily destroyed, and is difficult to keep its ultra-hydrophobicity in use.Prepare super-hydrophobic coat at present simultaneously
Method is typically more complicated, and process conditions are harsher, it is difficult to realize live large area coating.Therefore, invent it is a kind of floride-free and
Performance is stable, can post coat, simple and easy super-hydrophobic coat preparation and application method, to push super-hydrophobic coat in reality
Application in border production, life is of great significance and more practical value.
Graphene has excellent mechanical property, can construct stable nano-micro structure, but graphene chemical inertness, Wu Fahe
Organic siliconresin uniformly mixes on molecular scale, instead results in coating mechanical properties decrease；But the active oxidation of chemical property
Graphene hydrophily is too strong, causes coating hydrophobic effect bad.Currently used technical solution is will be at graphene oxide fluorination
Reason is to reduce its surface energy, but this can bring environmental problem as stated in the background art.In addition, existing prepare super-hydrophobic painting
The method of layer is typically more complicated, and process conditions are harsher, it is difficult to realize live large area coating.
Summary of the invention
That the purpose of the present invention is to provide a kind of floride-free and performances is stable, can post coat, simple and easy not fluorine-containing
Graphene-organic siliconresin super hydrophobic coating preparation method and application.Wherein, graphene provides excellent mechanical property and structure
Nano-micro structure is built, organic siliconresin provides splendid hydrophobic and film-formation result.
It is to solve the above-mentioned problems the technical scheme is that such: a kind of not fluorine-containing graphene-organosilicon tree
The preparation method of rouge super hydrophobic coating reacts with silane coupling agent first with the active graphene oxide of chemical property, makes graphite
Alkene surface silanization promotes the compatibility with organic siliconresin；The graphene of silanization is mixed with organic siliconresin again, is applied
Film, dry solidification obtain graphene-organic siliconresin super-hydrophobic coat.
Specifically includes the following steps:
A, disperse graphene oxide powder and silane coupling agent in solvent, stir and ultrasound to be allowed to evenly dispersed 0.5-7 small
The slurries filtration is drying to obtain silanization graphene by Shi Hou.
Wherein: solvent be one of organic solvents such as alcohol, ether, dimethyl acetamide, chloroform, N-Methyl pyrrolidone or
Several mixing of person.
Silane coupling agent be gamma-aminopropyl-triethoxy-silane, γ-(the third oxygen of 2,3- epoxy) propyl trimethoxy silicane,
N-(β-aminoethyl)-γ-aminopropyltriethoxy dimethoxysilane, N-(β-aminoethyl) one in-γ-aminopropyltrimethoxysilane
Kind or several mixing.
It counts in mass ratio, 1-10 parts of graphene oxide, 1~50 part of silane coupling agent, 10~2000 parts of solvent；
Preferably, graphene oxide 1-5 parts, 1~25 part of silane coupling agent, 30~500 parts of solvent；More preferably
It is 1-5 parts of graphene oxide, 1~30 part of silane coupling agent, 20~200 parts of solvent.
B, the silanization graphene in A is added in organosilicon, strong stirring is allowed to evenly dispersed, add solvent with
Viscosity is adjusted, graphene-organosilicon coating is obtained.
Wherein silanization graphene, organosilicon and solvent are counted in mass ratio, and 1-20 parts of silanization graphene, organosilicon 1~
100 parts, 50-3000 parts of solvent；
Organosilicon therein is mixing one or more of in hydroxy silicon oil, methoxyl group silicone oil, ethyoxyl silicone oil or alkyl silicic acids；
Solvent is ester, ether, ketone, alcohol, aromatic hydrocarbon, mixing one or more of in alkane.
Preferably, silanization graphene 1-10 parts, 1-20 parts of organosilicon, 100-2000 parts of solvent.
C, graphene-organosilicon coating in B is coated on substrate surface, be heating and curing, obtain graphene-organosilicon tree
Rouge super-hydrophobic coat.
Wherein heating temperature is 100-300 DEG C, and heating time is 1-24 hours；Preferably 120-200 DEG C of temperature, time
2-12 hours.
The substrate be metal material, inorganic non-metallic material (such as glass, ceramics), high molecular material (such as plastics),
The solid materials such as fabric or composite material.
Specifically, the present invention provides a kind of not fluorine-containing graphene-organosilicon tree hydrophobic coating preparation methods, including
Following steps:
1, it disperses graphene oxide powder and silane coupling agent in solvent D, stirs and ultrasound is allowed to evenly dispersed, then will
Mixture filtration drying obtains silanization graphene.
2, the silanization graphene in A is added in organosilicon, is strongly allowed to evenly dispersed, add solvent E to adjust
Viscosity is saved, graphene-organosilicon coating is obtained.
Further, the graphene oxide powder and silane coupling agent and solvent D, are counted, graphite oxide in mass ratio
1-10 parts of alkene, 1~50 part of silane coupling agent, D10-2000 parts of solvent；The silane coupling agent is gamma-aminopropyl-triethoxy silicon
Alkane, γ-(the third oxygen of 2,3- epoxy) propyl trimethoxy silicane, N-(β-aminoethyl)-γ-aminopropyltriethoxy dimethoxysilane or
N-(β-aminoethyl) mixing one or more of in-γ-aminopropyltrimethoxysilane；The solvent D is organic solvent, specifically
It can be mixing one or more of in alcohol, ether, dimethyl acetamide, chloroform, N-Methyl pyrrolidone.
Further, the silanization graphene and organosilicon are counted in mass ratio, and 1-20 parts of silanization graphene, organosilicon 1
~100 parts, 50-3000 parts of solvent E；The organosilicon be hydroxy silicon oil, containing hydrogen silicone oil, vinyl silicone oil, in ethyoxyl silicone oil
One or more of mixing；Solvent E is ester, ether, ketone, alcohol, aromatic hydrocarbon, mixing one or more of in alkane.
Further, the graphene-organosilicon super hydrophobic coating is coated on substrate surface, be heating and curing to get graphite
Alkene-organic siliconresin super-hydrophobic coat.Wherein heating temperature is 100-300 DEG C, and heating time is 1-24 hours；The substrate is
Metal material, inorganic non-metallic material (such as glass, ceramics), high molecular material (such as plastics), fabric or composite material are solid
Body material.
Organic siliconresin is that a kind of alternately linked by silicon atom and oxygen atom forms skeleton, then by different organic groups with
The general designation of the polymer of silicon atom connection.Due to the unique texture of organosilicon, the performance of inorganic material and organic material has been had both,
In addition to the fundamental propertys such as low with surface tension, viscosity-temperature coefficient is small, compressibility is high, gas permeability is high, also have high-low temperature resistant,
The excellent characteristics such as electric insulation, resistance to oxidation stability, weatherability, fire retardant, hydrophobic, corrosion-resistant, non-toxic and tasteless and physiological inertia.
Wherein single-component silicon rubber is easy-to-use, has good adhesive property and solidfied material electrical insulation properties；Have simultaneously moisture-proof
The functions such as shockproof, arc resistant, ageing-resistant, moisture-proof.Graphene is a kind of novel carbon nanomaterial, has specific surface area height, connects
The features such as contacting surface product is big, superficial attractive forces are strong.
The beneficial effects of the present invention are: graphene and organic siliconresin, which are incorporated in substrate surface, forms two-dimension plane structure,
The adsorption capacity for enhancing coating and substrate, makes the more uniform densification of coating, and bond strength is higher, improves the toughness, wear-resisting of coating
Property and antiseptic property.In addition, the unique two-dimensional slice structure of graphene helps to construct coarse nano-micro structure in coating surface,
In conjunction with the distinctive physical and chemical performance of organic siliconresin, the super-hydrophobic painting of excellent physical property and stable chemical performance is constructed
Layer.
Detailed description of the invention
Fig. 1 is the hydrophobicity experiment effect comparison diagram of glass material.
Left side is the hydrophobicity effect figure of simple glass；Right side is to be coated with graphene-organic siliconresin super-hydrophobic coat
Sheet glass hydrophobicity effect figure.
Specific embodiment
The present invention will be described in further detail below with reference to the embodiments of the drawings.
In order to be easy to understand the technical means, the creative features, the aims and the efficiencies achieved by the present invention, tie below
Conjunction is specifically illustrating, and the present invention is further explained.
Embodiment 1, a kind of preparation method of not fluorine-containing graphene-organic siliconresin super hydrophobic coating
It disperses 10g graphene oxide powder and 10g gamma-aminopropyl-triethoxy-silane in 300g ethyl alcohol, stirs simultaneously ultrasound 1
Hour, filtration drying obtains silanization graphene.10g silanization graphene is added in 30g hydroxy silicon oil, strength mechanical stirring is extremely
Uniformly, 800g butyl acetate is added to adjust viscosity, is stirred evenly up to graphene-organic siliconresin super hydrophobic coating.It will
Graphene-organic siliconresin super hydrophobic coating sprays to glass pane surface, heated at 300 DEG C 1 hour it is organic to get graphene-
Silicone resin super-hydrophobic coat.(Fig. 1)
In all embodiments, in addition to using spraying method, blade coating, spin coating, drop coating, dip-coating, brushing etc. available can also be
What coating method.
Embodiment 2, a kind of preparation method of not fluorine-containing graphene-organic siliconresin super hydrophobic coating
By 10g graphene oxide powder, 10g γ-(2,3- the third oxygen of epoxy) propyl trimethoxy silicane is scattered in 500g dimethyl
In acetamide, stir and 2 hours ultrasonic, filtration drying obtains silanization graphene.30g methyl is added in 10g silanization graphene
In silicic acid and 70g hydroxy silicon oil, to uniform, add 200g hexane has strength mechanical stirring to adjust viscosity to get graphene-
Machine silicone resin super hydrophobic coating.Graphene-organic siliconresin super hydrophobic coating is brushed to silastic surface, is heated at 120 DEG C
24 hours to get graphene-organic siliconresin super-hydrophobic coat.
Embodiment 3, a kind of preparation method of not fluorine-containing graphene-organic siliconresin super hydrophobic coating
500g dimethyl is dispersed by 10g graphene oxide powder, 10gN-(β-aminoethyl)-γ-aminopropyltrimethoxysilane
In acetamide, stir and 3 hours ultrasonic, filtration drying obtains silanization graphene.30g ethoxy is added in 10g silanization graphene
In base silicone oil and 70g hydroxy silicon oil, strength mechanical stirring adds 200g hexamethylene to adjust viscosity, stirs evenly to uniform
Up to graphene-organic siliconresin super hydrophobic coating.Graphene-organic siliconresin super hydrophobic coating is brushed to aluminium oxide ceramics
Plate surface heats 15 hours to get graphene-organic siliconresin super-hydrophobic coat at 150 DEG C.
Embodiment 4, a kind of preparation method of not fluorine-containing graphene-organic siliconresin super hydrophobic coating
By 10g graphene oxide powder, 30g γ-(2,3- the third oxygen of epoxy) propyl trimethoxy silicane is scattered in 1000g toluene
In, it stirs and 4 hours ultrasonic, filtration drying obtains silanization graphene.50g ethyoxyl silicone oil is added in 10g silanization graphene
In 30g methane-siliconic acid, 800g toluene is added to adjust viscosity to uniform in strength mechanical stirring, is obtained graphene-organosilicon and is applied
Material.Graphene-organic siliconresin super hydrophobic coating is brushed to stainless steel surface, heats 6 hours at 180 DEG C to get graphene-
Organic siliconresin super-hydrophobic coat.
The above description of the embodiment is only used to help understand the method for the present invention and its core ideas.It should be pointed out that pair
For those skilled in the art, without departing from the principle of the present invention, the present invention can also be carried out
Some improvements and modifications, these improvements and modifications also fall within the scope of protection of the claims of the present invention.
The foregoing description of the disclosed embodiments enables those skilled in the art to implement or use the present invention.
Various modifications to these embodiments will be readily apparent to those skilled in the art, as defined herein
General Principle can be realized in other embodiments without departing from the spirit or scope of the present invention.Therefore, of the invention
It is not intended to be limited to the embodiments shown herein, and is to fit to and the principles and novel features disclosed herein phase one
The widest scope of cause.
Claims (9)
1. a kind of preparation method of not fluorine-containing graphene-organic siliconresin super hydrophobic coating, which is characterized in that including following step
It is rapid:
Step A, it disperses graphene oxide powder and silane coupling agent in solvent D, is uniformly dispersed, then filter mixture
Dry silanization graphene；
Step B, the silanization graphene in step A is added in organosilicon, is uniformly dispersed, it is viscous to adjust to add solvent E
Degree, obtains graphene-organosilicon syrup.
2. a kind of preparation method of not fluorine-containing graphene-organic siliconresin super hydrophobic coating according to claim 1,
It being characterized in that, the graphene oxide powder, silane coupling agent and solvent D are counted in mass ratio, and 1-10 parts of graphene oxide,
1~50 part of silane coupling agent, 10-2000 parts of solvent D.
3. a kind of preparation side of not fluorine-containing graphene-organic siliconresin super hydrophobic coating according to claim 1 or 2
Method, which is characterized in that the silane coupling agent is gamma-aminopropyl-triethoxy-silane, γ-(2,3- the third oxygen of epoxy) propyl front three
Oxysilane, N-(β-aminoethyl)-γ-aminopropyltriethoxy dimethoxysilane, N-(β-aminoethyl)-γ-aminopropyl trimethoxy
One or more of mixing in base silane.
4. a kind of preparation side of not fluorine-containing graphene-organic siliconresin super hydrophobic coating according to claim 1 or 2
Method, which is characterized in that the solvent D is organic solvent, specially alcohol, ether, dimethyl acetamide, chloroform, N- crassitude
One or more of mixing in ketone.
5. a kind of preparation method of not fluorine-containing graphene-organic siliconresin super hydrophobic coating according to claim 1,
Be characterized in that, the silanization graphene, organosilicon and solvent E in parts by mass, 1-20 parts of silanization graphene, organosilicon 1
~100 parts, 50-3000 parts of solvent E.
6. a kind of preparation side of not fluorine-containing graphene-organic siliconresin super hydrophobic coating according to claim 1 or 5
Method, which is characterized in that the organosilicon is hydroxy silicon oil, containing hydrogen silicone oil, vinyl silicone oil, one or more of in ethyoxyl silicone oil
Mixing.
7. a kind of preparation side of not fluorine-containing graphene-organic siliconresin super hydrophobic coating according to claim 1 or 5
Method, which is characterized in that the solvent E is ester, ether, ketone, alcohol, aromatic hydrocarbon, mixing one or more of in alkane.
8. a kind of application method of not fluorine-containing graphene-organic siliconresin super hydrophobic coating, it is characterised in that by claim
Graphene prepared by one of 1-7-organosilicon super hydrophobic coating is coated on substrate surface, is heating and curing organic to get graphene-
Silicone resin super-hydrophobic coat.
9. according to claim 8 a kind of without fluorine graphene-organosilicon super hydrophobic coating application method, feature exists
In the substrate is metal material, inorganic non-metallic material, high molecular material, fabric or composite material.
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| CN201810661685.2A CN109096913A (en) | 2018-06-25 | 2018-06-25 | A kind of preparation method and application of not fluorine-containing graphene-organic siliconresin super hydrophobic coating |
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| CN201810661685.2A CN109096913A (en) | 2018-06-25 | 2018-06-25 | A kind of preparation method and application of not fluorine-containing graphene-organic siliconresin super hydrophobic coating |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109881496A (en) * | 2019-02-12 | 2019-06-14 | 常州纳元新材料科技有限公司 | One kind constructing graphene bionic super-hydrophobic coating and its manufacture craft |
| CN115029065A (en) * | 2022-06-24 | 2022-09-09 | 厦门防水博士工程技术有限公司 | Roof weather-resistant hydrophobic self-cleaning coating and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107880305A (en) * | 2017-12-19 | 2018-04-06 | 中物院成都科学技术发展中心 | A kind of polymer composites of high air-liquid barrier property and preparation method thereof |
-
2018
- 2018-06-25 CN CN201810661685.2A patent/CN109096913A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107880305A (en) * | 2017-12-19 | 2018-04-06 | 中物院成都科学技术发展中心 | A kind of polymer composites of high air-liquid barrier property and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109881496A (en) * | 2019-02-12 | 2019-06-14 | 常州纳元新材料科技有限公司 | One kind constructing graphene bionic super-hydrophobic coating and its manufacture craft |
| CN115029065A (en) * | 2022-06-24 | 2022-09-09 | 厦门防水博士工程技术有限公司 | Roof weather-resistant hydrophobic self-cleaning coating and preparation method thereof |
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