CN109370370A - A kind of graphene exothermic paint and preparation method thereof - Google Patents
A kind of graphene exothermic paint and preparation method thereof Download PDFInfo
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- CN109370370A CN109370370A CN201811052072.5A CN201811052072A CN109370370A CN 109370370 A CN109370370 A CN 109370370A CN 201811052072 A CN201811052072 A CN 201811052072A CN 109370370 A CN109370370 A CN 109370370A
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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
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
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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
- C09D5/24—Electrically-conducting 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
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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
- C09D7/65—Additives macromolecular
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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
- C09D7/66—Additives characterised by particle size
- C09D7/67—Particle size smaller than 100 nm
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- 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
- C08K3/38—Boron-containing compounds
- C08K2003/387—Borates
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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
- C08K2201/00—Specific properties of additives
- C08K2201/001—Conductive additives
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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
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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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
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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Abstract
The present invention relates to a kind of graphene exothermic paints and preparation method thereof.The present invention includes following components by weight percentage: graphene 2%-7%, diluent 20%-40%, dispersing agent 0.15%-2%, epoxy resin 20%-40%, curing agent 1.6%-6.6%, filler 10%-50%, coupling agent 0.2%-1%, the fineness of graphene exothermic paint is 30-60 μm, solid content 30-60%.Graphene exothermic paint of the invention has excellent comprehensive performance, strong to the adhesive force of substrate, is prepared into after heating film, it can be achieved that integral face generates heat, heating property is good, and bending performance is strong, and working life is significantly promoted.The present invention has uniform fineness and suitable solid content, and after being prepared into heating film, the appearance of heating film is good, unit coating area is larger, at low cost.The present invention can be produced and be applied in the preparation of heating film by simple step.
Description
Technical field
The present invention relates to a kind of graphene exothermic paints and preparation method thereof.
Background technique
Winter warming problem along the Changjiang river areas to the south annoyings always government and general public.Due to such area
There is no central heating, people can only use domestic air conditioning or electric heating floor of mating formation to carry out warming for many years.However, these take
Warm mode largely passes through traditional wire heat-emitting products and generates heat, and at high cost, power consumption is big, fever is uneven, and heating effect is unsatisfactory.
Graphene is a kind of two-dimensional carbon nanomaterial, with excellent electric heating property by extensive concern.Graphene hair
Hot coating is nontoxic, secure persistent, function admirable.Graphene exothermic paint is prepared into heating film, it is whole uniform after energization
Fever, can overcome traditional heat-emitting products power consumption big, non-uniform disadvantage of generating heat.However, current graphene exothermic paint is still
Right Shortcomings, for example, graphene coating it is weak to substrate adhesive force, when being prepared into the unstable heating effect after heating film, heating
Between it is long, bending performance is poor, working life is short the problems such as all limit further applying for graphene exothermic paint.
Summary of the invention
In view of the deficiencies of the prior art, the purpose of the present invention is to provide a kind of exothermic paint of graphene and its preparation sides
Method.Graphene exothermic paint of the invention has excellent comprehensive performance, strong to the adhesive force of substrate, after being prepared into heating film,
Integral face fever can be achieved, heating property is good, and bending performance is strong, and working life is significantly promoted.
The invention adopts the following technical scheme:
A kind of graphene exothermic paint, including following components by weight percentage:
The fineness of the graphene exothermic paint is 30-60 μm, solid content 30-60%.
Preferably, the graphene is prepared by full liquid physics stripping method；The number of plies of the graphene is 1-9
Layer.
Preferably, the diluent is one of toluene, dimethylbenzene, isopropanol, n-butanol, acetone or a variety of.
Preferably, the dispersing agent is polyvinylpyrrolidone, propylene glycol methyl ether acetate, polyether carbonate, poly- third
One of olefin(e) acid ester is a variety of.
Preferably, the epoxy resin is one of epoxy resin 901-75, epoxy resin 128, epoxy resin 144
Or it is a variety of.
Preferably, the curing agent is one of aromatic polyamine, organic acid anhydride, methylimidazole or a variety of；Institute
The aromatic polyamine stated is diaminodiphenylsulfone；The organic acid anhydride is maleic anhydride, one in phthalic anhydride
Kind.
Preferably, the filler is one of graphene, carbon nanotube, superconductive carbon black, tourmaline powder or a variety of.
Preferably, the coupling agent is one of epoxy-modified silane, organic acid, amino modified organic acid or more
Kind；The epoxy-modified silane is amino modified alkoxy polysiloxane, epoxy-modified more alkoxy polysiloxanes.
The preparation method of above-mentioned graphene exothermic paint, comprising the following steps:
(1) ultrasonic disperse processing is carried out to graphene；
(2) step (1) treated graphene, diluent, dispersant is uniform, form graphene dispersing solution；
(3) epoxy resin, curing agent, filler, coupling agent are uniformly mixed with graphene dispersing solution, form mixture；
(4) abrasive lapping will be mixed, obtaining fineness is 30-60 μm, and solid content is the graphene exothermic paint of 30-60%.
Above-mentioned graphene exothermic paint is applied to be prepared into heating film, comprising the following steps:
(1) graphene exothermic paint is uniformly coated to PI film by 50 μm of bar spreader, forms heating film half
Finished product；
(2) heating film semi-finished product dry 10min at 120 DEG C of temperature to get heating film is arrived.
Graphene of the invention is prepared by full liquid physics stripping method.
More specifically, the method that full liquid water phase physics removing prepares graphene, comprising the following steps:
(1) using ultrapure water to impregnate carbon content is 99.99%, and dilation is 200 times of expanded graphite, carries out wetting immersion
Processing, for 8-15mL:1g, the time for soaking immersion treatment is 18- for the volume of the ultrapure water used and the mass ratio of expanded graphite
25h；
(2) expanded graphite after wetting immersion treatment in step (1) is put into sand mill stirring, placed at colloid mill
Reason, obtains expanded graphite soak, wherein the concrete operations of milled processed are as follows: puts the expanded graphite after wetting immersion treatment
Entering stir process 1.5-4h in the sand mill equipped with a small amount of zirconium pearl, the revolving speed of sand mill is set as 1000-2000rad/min, then
It is put into milling treatment of colloid 3-6h, the power of colloid mill is 1-2kW, treating capacity 18-25L/h；
(3) the expanded graphite soak in step (2) is put into high pressure homogenizer and carries out high-pressure homogeneous processing, then with height
The processing of emulsification pretreatment pump, then handled with super-pressure critical assembly, obtain graphene dispersing solution, wherein the item of high-pressure homogeneous processing
Part are as follows: time 1.5-3h, pressure 50-100MPa, the time of emulsification treatment are 2.5-5h, the condition of the critical processing of super-pressure
Are as follows: time 2.5-5h, pressure 120-180MPa；
(4) step (3) are handled to obtained graphene dispersing solution stratification, are done by spraying at being 180-250 DEG C in temperature
It is dry to get arrive graphene.
The graphene lattice structure being prepared using full liquid physics stripping method is complete, simultaneously containing a small amount of-OH etc.
Hydrophilic radical has preferable dispersion performance, specific surface area 679m2/ g, graphene carbon content are 99.99wt%, metal
Ion concentration≤100ppm, thermal coefficient are 3800W/ (mK).
Beneficial effects of the present invention:
(1) present invention can make graphene and filler preferably build conductive network by ultrasonic disperse graphene；Graphite
Alkene exothermic paint joined the filler of high tret, help to reduce resistance of the invention；Present invention employs specific idols simultaneously
Join agent, had both increased the present invention to the adhesive force of filler, and reduced the phenomenon that losing powder in use process, and also enhanced the present invention to base
The adhesive force of material；
(2) graphene exothermic paint of the invention has excellent heating property, is prepared into after heating film, it can be achieved that whole
Face fever, heating power consumption is low, and resistance to low temperature is good, and the heating-up time is short, and heating temperature is high；Bending is strong simultaneously, long working life；
(3) graphene exothermic paint of the invention has uniform fineness and suitable solid content, is prepared into heating film
Afterwards, the appearance of heating film is good, unit coating area is larger, at low cost；
(4) graphene exothermic paint preparation process of the invention is simple, easy to operate, can be applied to by simple step
In the preparation of heating film.
Specific embodiment
Below by embodiment, the present invention will be described in detail.
Embodiment 1
A kind of graphene exothermic paint, including following components by weight percentage:
The fineness of graphene exothermic paint is 40 μm, solid content 55.8%.
The preparation method of above-mentioned graphene exothermic paint, comprising the following steps:
(1) ultrasonic disperse is carried out to graphene；
(2) step (1) treated graphene, toluene, isopropanol, polyvinylpyrrolidone are added in blender and are stirred
30min, mixing speed 1000r/min are mixed, graphene dispersing solution is formed；
(3) by epoxy resin 901-75, methylimidazole, superconductive carbon black, amino modified alkoxy polysiloxane and stone
Black alkene dispersion liquid is mixed, mixing speed 1000r/min, forms mixture；
(4) abrasive lapping will be mixed by grinder, and will be 40 μm when mixture reaches fineness, solid content 55.8%.To obtain the final product
To graphene exothermic paint.
Embodiment 2
A kind of graphene exothermic paint, including following components by weight percentage:
The fineness of graphene exothermic paint is 40 μm, solid content 55.5%.
The preparation method of above-mentioned graphene exothermic paint, comprising the following steps:
(1) ultrasonic disperse is carried out to graphene；
(2) step (1) treated graphene, dimethylbenzene, isopropanol, propylene glycol methyl ether acetate are added to blender
Middle stirring 30min, mixing speed 1000r/min form graphene dispersing solution；
(3) by epoxy resin 901-75, methylimidazole, carbon nanotube, epoxy-modified more alkoxy polysiloxanes and stone
Black alkene dispersion liquid is mixed, mixing speed 1000r/min, forms mixture；
(4) abrasive lapping will be mixed by grinder, and will be 40 μm when mixture reaches fineness, solid content 55.5%.To obtain the final product
To graphene exothermic paint.
Embodiment 3
A kind of graphene exothermic paint, including following components by weight percentage:
The fineness of graphene exothermic paint is 40 μm, solid content 54.9%.
The preparation method of above-mentioned graphene exothermic paint, comprising the following steps:
(1) ultrasonic disperse is carried out to graphene；
(2) step (1) treated graphene, dimethylbenzene, isopropanol, polyether carbonate are added in blender and are stirred
30min, mixing speed 1000r/min form graphene dispersing solution；
(3) by epoxy resin 128, diaminodiphenylsulfone, tourmaline powder, epoxy-modified more alkoxy polysiloxanes and graphite
Alkene dispersion liquid is mixed, mixing speed 1000r/min, forms mixture；
(4) abrasive lapping will be mixed by grinder, and will be 40 μm when mixture reaches fineness, solid content 54.9%.To obtain the final product
To graphene exothermic paint.
Embodiment 4
A kind of graphene exothermic paint, including following components by weight percentage:
The fineness of graphene exothermic paint is 40 μm, solid content 54.5%.
The preparation method of above-mentioned graphene exothermic paint, comprising the following steps:
(1) ultrasonic disperse is carried out to graphene；
(2) step (1) treated graphene, isopropanol, acetone, polyvinylpyrrolidone are added in blender and are stirred
30min, mixing speed 1000r/min are mixed, graphene dispersing solution is formed；
(3) by epoxy resin 901-75, methylimidazole, superconductive carbon black, epoxy-modified more alkoxy polysiloxanes with
Graphene dispersing solution is mixed, mixing speed 1000r/min, forms mixture；
(4) abrasive lapping will be mixed by grinder, and will be 40 μm when mixture reaches fineness, solid content 54.5%.To obtain the final product
To graphene exothermic paint.
Comparative example 1
A kind of graphene exothermic paint, including following components by weight percentage:
The fineness of graphene exothermic paint is 40 μm, solid content 55.8%.
The preparation method of above-mentioned graphene exothermic paint, comprising the following steps:
(1) ultrasonic disperse is carried out to graphene；
(2) step (1) treated graphene, dimethylbenzene, n-butanol, polyacrylate are added in blender and are stirred
30min, mixing speed 1000r/min form graphene dispersing solution；
(3) by epoxy resin 144, methylimidazole, tourmaline powder, amino modified alkoxy polysiloxane and graphene point
Dispersion liquid is mixed, mixing speed 1000r/min, forms mixture；
(4) abrasive lapping will be mixed by grinder, and will be 40 μm when mixture reaches fineness, solid content 55.8%.To obtain the final product
To graphene exothermic paint.
Comparative example 2
A kind of exothermic paint, including following components by weight percentage:
The fineness of exothermic paint is 40 μm, solid content 54.7%.
The preparation method of above-mentioned exothermic paint, comprising the following steps:
(1) toluene, isopropanol, polyvinylpyrrolidone are added in blender and stir 30min, mixing speed is
1000r/min forms dispersion liquid；
(2) by epoxy resin 901-75, methylimidazole, superconductive carbon black, epoxy-modified more alkoxy polysiloxanes with
Dispersion liquid is mixed, mixing speed 1000r/min, forms mixture；
(3) abrasive lapping will be mixed by grinder, and will be 40 μm when mixture reaches fineness, solid content 54.7%.To obtain the final product
To exothermic paint.
Experimental example 1
The exothermic paint of embodiment 1-4, the graphene exothermic paint of comparative example 1, comparative example 2 is prepared into heating film, it is right
Fever film properties are tested, and test result is as shown in table 1:
The fever film properties test of table 1
As known from Table 1, the bending performance of the heating film as obtained by the graphene exothermic paint of embodiment 1-4, low temperature resistant
Performance all has many advantages, such as to be obviously improved, and with the heating-up time is short, heating temperature is high, resistance is low, long working life.Implement
In example, when the additive amount of graphene is 5%, obtained heating film when input voltage is 5V with excellent comprehensive performance,
Folding 1000 times or more does not still influence the use of product, suitable for wearable product.Adhesive force of the invention power at
Film object is related with the proportion of filler, such as the pigment of coating；Also related with the polarity of substrate, the type of coupling agent；Of the invention
Heating-up time is mainly influenced by resistance, and the size of resistance is related with the proportion of film forming matter and graphene, filler, due to film forming matter
It is insulation, graphene and filler are conductive, therefore the graphene of different ratio, filler will lead to the resistance difference of product,
The heating property for also resulting in product is different.The present invention prepares performance by the way that different materials is selected and matched
Suitable product.
Above embodiments do not have point of superiority and inferiority, only use different formulas according to the different market demands, obtain difference
The product of performance.
Claims (10)
1. a kind of graphene exothermic paint, which is characterized in that including following components by weight percentage:
The fineness of the graphene exothermic paint is 30-60 μm, solid content 30-60%.
2. graphene exothermic paint according to claim 1, which is characterized in that the graphene passes through full liquid physics
Stripping method preparation；The number of plies of the graphene is 1-9 layers.
3. graphene exothermic paint according to claim 1, which is characterized in that the diluent be toluene, dimethylbenzene,
One of isopropanol, n-butanol, acetone are a variety of.
4. graphene exothermic paint according to claim 1, which is characterized in that the dispersing agent is polyvinylpyrrolidine
One of ketone, propylene glycol methyl ether acetate, polyether carbonate, polyacrylate are a variety of.
5. graphene exothermic paint according to claim 1, which is characterized in that the epoxy resin is epoxy resin
One of 901-75, epoxy resin 128, epoxy resin 144 are a variety of.
6. graphene exothermic paint according to claim 1, which is characterized in that the curing agent be aromatic polyamine,
One of organic acid anhydride, methylimidazole are a variety of；The aromatic polyamine is diaminodiphenylsulfone；The organic acid
Acid anhydride is one of maleic anhydride, phthalic anhydride.
7. graphene exothermic paint according to claim 1, which is characterized in that the filler is graphene, carbon nanometer
One of pipe, superconductive carbon black, tourmaline powder are a variety of.
8. graphene exothermic paint according to claim 1, which is characterized in that the coupling agent is epoxy-modified silicon
One of alkane, organic acid, amino modified organic acid are a variety of；The epoxy-modified silane is poly- for amino modified alkoxy
Siloxanes, epoxy-modified more alkoxy polysiloxanes.
9. the preparation method of graphene exothermic paint of any of claims 1-8, which is characterized in that including following step
It is rapid:
(1) ultrasonic disperse processing is carried out to graphene；
(2) step (1) treated graphene, diluent, dispersant is uniform, form graphene dispersing solution；
(3) epoxy resin, curing agent, filler, coupling agent are uniformly mixed with graphene dispersing solution, form mixture；
(4) abrasive lapping will be mixed, obtaining fineness is 30-60 μm, and solid content is the graphene exothermic paint of 30-60%.
10. graphene exothermic paint of any of claims 1-8 is applied to be prepared into heating film.
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| CN109942935A (en) * | 2019-03-07 | 2019-06-28 | 中山市君泽科技有限公司 | Graphene-based conductive, the graphene-based power regulation particle of one kind and preparation method |
| CN111432508A (en) * | 2020-04-15 | 2020-07-17 | 威海无缝新材料有限公司 | Graphene fast heating film and preparation method thereof |
| CN112375462A (en) * | 2020-11-26 | 2021-02-19 | 广东航科新材料有限公司 | Graphene electric heating slurry and preparation method thereof |
| CN112694774A (en) * | 2021-01-21 | 2021-04-23 | 湖南翰坤实业有限公司 | Environment-friendly energy-saving nano graphene heating coating and preparation method thereof |
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| CN109942935A (en) * | 2019-03-07 | 2019-06-28 | 中山市君泽科技有限公司 | Graphene-based conductive, the graphene-based power regulation particle of one kind and preparation method |
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| CN112694774A (en) * | 2021-01-21 | 2021-04-23 | 湖南翰坤实业有限公司 | Environment-friendly energy-saving nano graphene heating coating and preparation method thereof |
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