CN105505134A - Graphene conductive coating and preparation method thereof - Google Patents

Graphene conductive coating and preparation method thereof Download PDF

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Publication number
CN105505134A
CN105505134A CN201510896301.1A CN201510896301A CN105505134A CN 105505134 A CN105505134 A CN 105505134A CN 201510896301 A CN201510896301 A CN 201510896301A CN 105505134 A CN105505134 A CN 105505134A
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graphene
conductive coating
preparation
graphene conductive
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岳巍
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Nantong Jinyuan Intelligent Technology Co Ltd
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Nantong Jinyuan Intelligent Technology Co Ltd
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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
    • C09D163/10—Epoxy resins modified by unsaturated compounds
    • 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
    • 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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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Paints Or Removers (AREA)
  • Carbon And Carbon Compounds (AREA)

Abstract

The invention discloses a graphene conductive coating and a preparation method thereof. The graphene conductive coating is prepared from graphene, epoxy acrylic resin, polyurethane acrylate, polyethylene wax and ethyl alcohol, and is prepared by technologies such as ultrasonic dispersion, mechanical agitation and the like. The graphene conductive coating has the advantages of being good in conductivity, heat conduction property and circuit substrate bonding performance, less in pollution, environment-friendly, low in cost, suitable for large-scale industrial production and the like; the graphene conductive coating has wide application prospect in the fields such as high-power light-emitting diode (LED) substrates, flat panel displays, solar cell preparation and the like which have requirements on the high-performance and low-cost conductive coating.

Description

A kind of graphene conductive coating and preparation method thereof
Technical field
The present invention relates to a kind of electrically conducting coating, be specially a kind of graphene conductive coating and preparation method thereof.
Background technology
Along with the development of energy-conserving and environment-protective and information industry, electrically conducting coating is day by day vigorous in the demand in the fields such as high power LED substrate, flat-panel monitor, solar panel.Although better with the conventional conductive coating conductivity adding silver powder, copper powder, the silver-colored electrically conducting coating of nickel powder, copper electrically conducting coating, nickel electrically conducting coating are representative, owing to wherein with the addition of the precious metal materials such as silver, this improves the manufacturing cost of coating undoubtedly.
Another developing direction of electrically conducting coating is the filler using carbon material as coating, prepares the electrically conducting coating of high conduction performance.Due to carbon material, as Graphite Powder 99, carbon fiber etc., as conductive filler material, wide material sources and price comparatively noble metal powder are cheap, have vast potential for future development.
Graphene, as new carbon, is with sp by carbon atom 2the two-dimension nano materials only with 1 atomic layer level thickness of hybridized orbital composition, its room temperature resistivity is 10 -6Ω cm, the argent minimum than resistivity during room temperature is also low, and the current density patience of Graphene is good, reaches 0.2 × 10 9a/cm 2(being 100 times of copper), Graphene has unique carrier properties in addition, has surprising high electron mobility (1.5 × 10 under room temperature 4cm 2v -1s -1).Meanwhile, the thermal conductivity of Graphene is (4.54 ~ 5.30) × 10 3wm -1k -1, being significantly improved compared with Single Walled Carbon Nanotube, multi-walled carbon nano-tubes, is 3 times of pure diamond under room temperature, 12 times of fine silver, 13 times of fine copper.
Due to the structure of the uniqueness that Graphene has, have both the conduction of above-mentioned excellence, heat conductivility, no matter from theory or experimental study aspect, it has shown great scientific research value and application advantage all in electrically conducting coating field.At present, existing related researcher expands research to graphene conductive coating, and as CN103131232A patent of invention discloses a kind of watersoluble plumbago alkene electrically conducting coating and preparation method thereof, this coating has application prospect in pcb board maintenance etc.CN10449377A patent of invention discloses a kind of Graphene coating electrically conducting coating and preparation method thereof, it is said that this coating has application prospect in fields such as flat-panel monitors.
But because the development of graphene conductive coating is in the starting stage, many problems are also had to need to solve, contain strong acid or strong oxidizer as in published graphene conductive coating more, environment friendly is poor, coating composition is complicated, meanwhile, the preparation technology of coating is more complicated, industrialization difficulty is high and cost is high.
Summary of the invention
For the multiple technologies problem existed in current graphene conductive coating, for expanding the Application Areas of graphene conductive coating, exploitation integrates the graphene conductive coating of multiple premium properties, this application provides a kind of graphene conductive coating and preparation method thereof.
For achieving the above object, the application is by the following technical solutions:
A kind of graphene conductive coating, by massfraction, described coating comprises: Graphene 14 ~ 18 parts, Epocryl 14 ~ 18 parts, urethane acrylate 6 ~ 7 parts, polyethylene wax 5 ~ 6 parts, ethanol 25 ~ 40 parts.
First preferred version of graphene conductive coating, Graphene is the combination of single-layer graphene, multi-layer graphene or two kinds of Graphene different contents, and the lamellar spacing of Graphene is not more than 3nm.
A preparation method for graphene conductive coating, comprises following steps:
1) Graphene is added in ethanol, use ultrasonic wave to be disperseed in ethanol by Graphene with setting power and setting-up time, obtain Graphene ethanolic soln;
2) Epocryl, urethane acrylate, polyethylene wax are joined step 1) in obtain Graphene ethanolic soln in, use mechanical stirring, with the time of the rotating speed of setting and setting, above-mentioned mixed solution is disperseed, the graphene conductive coating described in acquisition.
First preferred version of the preparation method of graphene conductive coating, hyperacoustic power is 200 ~ 4000W, and the time of ultrasonic wave dispersion is 15 ~ 60min.
Second preferred version of the preparation method of graphene conductive coating, churned mechanically rotating speed is 300 ~ 1500rpm, and the churned mechanically time is 15 ~ 60min.
3rd preferred version of the preparation method of graphene conductive coating, urethane acrylate prepares gained by following methods, whole reaction under nitrogen protection, under 70 DEG C of conditions, in there-necked flask, add hexamethylene diisocyanate and 1-Methoxy-2-propyl acetate, drip terminal hydroxy group fluorine cpd, after dropwising with the speed of 3 ~ 5mL/min, continue stirring reaction 2.5 hours, obtain the first intermediate; Under 80 DEG C of conditions, in the first intermediate, add 1-Methoxy-2-propyl acetate and catalyzer, then add end hydroxypropyl polydimethylsiloxane and polyoxyethylene glycol, react 3 hours, obtain the second intermediate; In the second intermediate, add 1-Methoxy-2-propyl acetate and stopper, then add terminal hydroxy group acrylate, continue reaction 2 hours, obtain urethane acrylate.
With immediate prior art ratio, graphene conductive coating of the present invention have conduction/good heat conductivity, coating composition comparatively simple, low without the compositions such as strong acid, highly basic or strong oxidizer, environmental friendliness, cost, be suitable for the advantages such as large-scale industrial production, have the field of demand to have broad application prospects at high power LED substrate, flat-panel monitor, solar panel etc. to high-performance, low cost electrically conducting coating.
Embodiment
Below in conjunction with embodiment, be clearly and completely described technical scheme of the present invention, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtained under creative work prerequisite, belong to the scope of protection of the invention.
Prepare urethane acrylate: whole reaction under nitrogen protection, under 70 DEG C of conditions, hexamethylene diisocyanate and 1-Methoxy-2-propyl acetate is added in there-necked flask, terminal hydroxy group fluorine cpd are dripped with the speed of 3 ~ 5mL/min, after dropwising, continue stirring reaction 2.5 hours, obtain the first intermediate; Under 80 DEG C of conditions, in the first intermediate, add 1-Methoxy-2-propyl acetate and catalyzer, then add end hydroxypropyl polydimethylsiloxane and polyoxyethylene glycol, react 3 hours, obtain the second intermediate; In the second intermediate, add 1-Methoxy-2-propyl acetate and stopper, then add terminal hydroxy group acrylate, continue reaction 2 hours, obtain urethane acrylate.
Embodiment 1:
Get Graphene 140g, Epocryl 180g, urethane acrylate 60g, polyethylene wax 60g and 250g ethanol.
The preparation method of graphene conductive coating:
1) add in 250g ethanol by 140g Graphene, use ultrasonic wave to be disperseed in ethanol by Graphene, ultrasonic power is 200W, and ultrasonic dispersing time is 15min, obtains Graphene ethanolic soln;
2) 180g Epocryl, 60g urethane acrylate, 70g polyethylene wax are joined step 1) in obtain Graphene ethanolic soln in, mechanical stirring oar is used to be disperseed, mechanical stirring rotating speed is 1500rpm, the mechanical stirring time is 60min, the graphene conductive coating described in final acquisition.
This graphene conductive coating is 2 × 10 through the conductive film resistivity that coating process obtains -3Ω cm.
Embodiment 2:
Get Graphene 160g, Epocryl 150g, urethane acrylate 65g, polyethylene wax 55g and 300g ethanol.
The preparation method of graphene conductive coating:
1) add in 300g ethanol by 160g Graphene, use ultrasonic wave to be disperseed in ethanol by Graphene, ultrasonic power is 2000W, and ultrasonic dispersing time is 30min, obtains Graphene ethanolic soln;
2) 150g Epocryl, 65g urethane acrylate, 55g polyethylene wax are joined step 1) in obtain Graphene ethanolic soln in, mechanical stirring oar is used to be disperseed, mechanical stirring rotating speed is 800rpm, the mechanical stirring time is 30min, the graphene conductive coating described in final acquisition.
This graphene conductive coating is 7 × 10 through the conductive film resistivity that coating process obtains -3Ω cm.
Embodiment 3:
Get Graphene 180g, Epocryl 140g, urethane acrylate 70g, polyethylene wax 50g and 400g ethanol.
The preparation method of graphene conductive coating:
1) add in 400g ethanol by 180g Graphene, use ultrasonic wave to be disperseed in ethanol by Graphene, ultrasonic power is 4000W, and ultrasonic dispersing time is 60min, obtains Graphene ethanolic soln;
2) 140g Epocryl, 70g urethane acrylate, 50g polyethylene wax are joined step 1) in obtain Graphene ethanolic soln in, mechanical stirring oar is used to be disperseed, mechanical stirring rotating speed is 300rpm, the mechanical stirring time is 15min, the graphene conductive coating described in final acquisition.
This graphene conductive coating is 6 × 10 through the conductive film resistivity that coating process obtains -4Ω cm.
Above embodiment is only in order to illustrate that technical scheme of the present invention is not intended to limit; those of ordinary skill in the field are to be understood that; can modify to the specific embodiment of the present invention with reference to above-described embodiment or equivalent to replace, these do not depart from any amendment of spirit and scope of the invention or equivalently to replace within the claims that all awaits the reply in application.

Claims (6)

1. a graphene conductive coating, is characterized in that, by massfraction, described coating comprises: Graphene 14 ~ 18 parts, Epocryl 14 ~ 18 parts, urethane acrylate 6 ~ 7 parts, polyethylene wax 5 ~ 6 parts, ethanol 25 ~ 40 parts.
2. graphene conductive coating according to claim 1, is characterized in that, described Graphene is the combination of single-layer graphene, multi-layer graphene or two kinds of Graphene different contents, and the lamellar spacing of Graphene is not more than 3nm.
3. the preparation method of a kind of graphene conductive coating according to claim 1, it is characterized in that, the preparation of described coating comprises following steps:
1) Graphene is added in ethanol, use ultrasonic wave to be disperseed in ethanol by Graphene with setting power and setting-up time, obtain Graphene ethanolic soln;
2) Epocryl, urethane acrylate, polyethylene wax are joined step 1) in obtain Graphene ethanolic soln in, use mechanical stirring, with the time of the rotating speed of setting and setting, above-mentioned mixed solution is disperseed, the graphene conductive coating described in acquisition.
4. the preparation method of graphene conductive coating according to claim 3, is characterized in that, described hyperacoustic power is 200 ~ 4000W, and the time of ultrasonic wave dispersion is 15 ~ 60min.
5. the preparation method of graphene conductive coating according to claim 3, is characterized in that, described churned mechanically rotating speed is 300 ~ 1500rpm, and the churned mechanically time is 15 ~ 60min.
6. the preparation method of graphene conductive coating according to claim 3, it is characterized in that, described urethane acrylate prepares gained by following methods, whole reaction under nitrogen protection, under 70 DEG C of conditions, adds hexamethylene diisocyanate and 1-Methoxy-2-propyl acetate in there-necked flask, terminal hydroxy group fluorine cpd are dripped with the speed of 3 ~ 5mL/min, after dropwising, continue stirring reaction 2.5 hours, obtain the first intermediate; Under 80 DEG C of conditions, in the first intermediate, add 1-Methoxy-2-propyl acetate and catalyzer, then add end hydroxypropyl polydimethylsiloxane and polyoxyethylene glycol, react 3 hours, obtain the second intermediate; In the second intermediate, add 1-Methoxy-2-propyl acetate and stopper, then add terminal hydroxy group acrylate, continue reaction 2 hours, obtain urethane acrylate.
CN201510896301.1A 2015-12-08 2015-12-08 Graphene conductive coating and preparation method thereof Pending CN105505134A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116875177A (en) * 2023-07-02 2023-10-13 江西金桥德克新材料有限公司 Electron beam curing self-cleaning coating for automobile surface and preparation method thereof

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103992460A (en) * 2014-06-11 2014-08-20 湖南本安亚大新材料有限公司 Urethane acrylate oligomer, preparation method of urethane acrylate oligomer, and coating prepared from urethane acrylate oligomer
CN104194455A (en) * 2014-08-25 2014-12-10 鸿纳（东莞）新材料科技有限公司 Graphene coating as well as preparation method and coating method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103992460A (en) * 2014-06-11 2014-08-20 湖南本安亚大新材料有限公司 Urethane acrylate oligomer, preparation method of urethane acrylate oligomer, and coating prepared from urethane acrylate oligomer
CN104194455A (en) * 2014-08-25 2014-12-10 鸿纳（东莞）新材料科技有限公司 Graphene coating as well as preparation method and coating method thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
张洪涛等: "《聚合物胶乳配方与应用》", 31 January 2008, 化学工业出版社 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116875177A (en) * 2023-07-02 2023-10-13 江西金桥德克新材料有限公司 Electron beam curing self-cleaning coating for automobile surface and preparation method thereof

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Application publication date: 20160420