CN103131232B - High-performance aqueous graphene paint and preparation method thereof - Google Patents
High-performance aqueous graphene paint and preparation method thereof Download PDFInfo
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- CN103131232B CN103131232B CN201310102556.7A CN201310102556A CN103131232B CN 103131232 B CN103131232 B CN 103131232B CN 201310102556 A CN201310102556 A CN 201310102556A CN 103131232 B CN103131232 B CN 103131232B
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Abstract
The invention discloses high-performance aqueous graphene paint and a preparation method thereof. The preparation method of the high-performance aqueous graphene paint comprises the following steps of: oxidizing natural graphite in an oxidant, adopting a two-step chemical reduction method to obtain organic molecule-modified graphene aqueous solution; and adding polyester, a neutralizing agent, a flatting agent, an antifoaming agent, a cross-linking agent and a catalyst by adopting a solution co-mixing method to obtain aqueous graphene paint. A conductive coating with high conductive performance and mechanical performance is obtained by carrying out spray-coating, ink-jet printing and printing on the obtained paint, the conductive coating can be applied to the field such as electromagnetic shielding, static electricity preventing, corrosion preventing, radiating, wear-resisting and electronic circuits, and therefore, the application value is extensive.
Description
Technical field
The present invention relates to a kind of watersoluble plumbago alkene electrically conducting coating and its manufacture method.
Background technology
Electrically conducting coating is applied on the grounds such as non-conductive polymer material, make it a kind of new type functional coating that there is conduction current and get rid of accumulate static charge ability, specific conductivity after film is generally greater than 10S/m, be widely applied to every field at present, the conduction as integrated circuit component connect, connect nonweldable place, shielding high frequency magnetic field plastic stent, airplane hidden material, conductive film etc.In addition, electrically conducting coating also has very large use value in electronic market, as design and reparation, automobile demist heating wire broken line repairing, the repairing of keyboard printed wiring etc. of PCB.
Current electrically conducting coating can be divided into structural conductive coating and addition type electrically conducting coating according to electrical conduction mechanism and composition.Structural conductive coating mainly has conducting function film with superpolymer self and is formed; Addition type electrically conducting coating mainly adds the conducting particles with conductive capability in the superpolymer of insulation, makes to contact with each other between conducting particles, form conductive path, make electrically conducting coating have conductive capability after superpolymer solidification.It is simple, easy to operate, with low cost and can be coated on the advantages such as various surfaces of complex shape that addition type electrically conducting coating has equipment, and market range of application is wider.
Recently, addition type electrically conducting coating is because the field such as electromagnetic wave shielding, antistatic, anti-corrosion of metal, electronic circuit, electrode light reflecting material that can be widely used in achieves comparatively large very fast progress, in succession develop multiple strong electroconductibility electrically conducting coating, as conductive filler material mainly contains metal system (silver powder, copper powder, nickel powder etc.), glass/metal compound and charcoal system (graphite, carbon black) etc.But these electrically conducting coatings, the mechanical strength and the electric conductivity that prepare coating are difficult to improve, and the density of coating is comparatively large, and these problems limit its range of application greatly simultaneously.And the graphene conductive material that latest developments are got up, because the little (0.77mg/m of its density
2), mechanical strength large (Young's modulus is 1060Gpa, and intensity is the highest in test material, and reaching 130Gpa, is more than 100 times of steel).In addition, its carrier mobility reaches 200000cm
2v
-1s
-1, exceed more than 10 times of commercial silicon chip mobility, there is the electric conductivity (10 also higher than silver
6scm
-1).Thus, be expected to using Graphene as conductive filler material solve above-mentioned electrically conducting coating Problems existing, expand range of application and the field of electrically conducting coating widely.
Summary of the invention
The present invention is directed to that existing electrically conducting coating density is large, conductivity and mechanical property are difficult to the problem that simultaneously improves, provide a kind of high-performance water-based graphene conductive coating and preparation method thereof.
The present invention adopts following technical scheme to realize:
A kind of high-performance water-based graphene conductive coating, this electrically conducting coating is by high connductivity (electric conductivity >10
3cm/S) and the Graphene of high water stability (more than half a year not precipitating in aqueous) be conductive filler material composition.
The present invention provides a kind of preparation method of high-performance water-based graphene conductive coating simultaneously, and step is as follows:
(1) under condition of ice bath, 0.5 ~ 5.0g graphite is joined in the vitriol oil of 40ml ~ 60ml, violent stirring 30min; Further by 12 ~ 30g KMnO
4join in above-mentioned mixed solution, violent stirring 30min; Above-mentioned mixed solution is transferred in 30 DEG C of water-baths, slowly add 18 ~ 40gNaNO
3, stir 60min; Under agitation, 100 ~ 140ml deionized water is joined continuously in above-mentioned mixed solution, then transferred in the oil bath of 90 DEG C of temperature, stir the 30min time; Dropwise add 12 ~ 20mlH again
2o
2, continue reaction 40min ~ 80min until solution becomes glassy yellow from dark-brown;
(2) under agitation, in above-mentioned glassy yellow graphene oxide solution, add a certain amount of dispersing agent, drip the hydrazine hydrate solution of 15 ~ 45ml after dissolving, at 40 DEG C ~ 80 DEG C temperature, react 1h; In above-mentioned solution, drip 15 ~ 45ml also original reagent further, continue reaction 20 ~ 60min, obtain stable graphene aqueous solution;
(3) in the graphene aqueous solution of aforementioned stable, add a certain amount of waterborne polyester, neutralizing agent, flow agent, defoamer, linking agent, catalytic reagent successively, stir certain hour at a certain temperature, high-performance water-based graphene conductive coating can be obtained.
The preparation method of described watersoluble plumbago alkene electrically conducting coating, in step (2), dispersing agent is PVP, PVA, PEG or PEDOT:PSS; The concentration of aqueous solution of dispersing agent is 0.5 ~ 20wt%.
The preparation method of described watersoluble plumbago alkene electrically conducting coating, in step (2), going back original reagent is acetic acid or hydroiodic acid HI; Acetic acid aqueous solution concentration is 10 ~ 30wt%, and hydriodic acid aqueous solution concentration is 10 ~ 40wt%.
The preparation method of described watersoluble plumbago alkene electrically conducting coating, in step (3), described waterborne polyester is, neutralizing agent is ethanolamines, and flow agent is only son's ethers, and defoamer is defoamer 901 or 902.
The preparation method of described watersoluble plumbago alkene electrically conducting coating, described waterborne polyester, neutralizing agent, flow agent, defoamer consumption are respectively 5 ~ 20wt%, 0.1 ~ 2wt%, 0.15 ~ 0.5wt%, the 0.02 ~ 0.1wt% of coating composition.
The preparation method of described watersoluble plumbago alkene electrically conducting coating, described linking agent is melamino-formaldehyde or aminoresin class, and add-on is 5 ~ 25wt% of waterborne polyester.
The preparation method of described watersoluble plumbago alkene electrically conducting coating, described catalytic reagent is ethylenediamines, and add-on is 0 ~ 2.0wt% of waterborne polyester.
The preparation method of described watersoluble plumbago alkene electrically conducting coating, described coating whipping temp is 5 ~ 30 DEG C, and churning time is 10min ~ 3 hour.
The purposes of watersoluble plumbago alkene electrically conducting coating prepared by described method: this coating is used for spraying, spray ink Printing and typography and prepares coating; This coating be used in macromolecular material, metallic substance, ceramic surface, for electromagnetic shielding, antistatic, anticorrosion, heat radiation, wear-resisting and field of electronic circuitry.
The purposes of described watersoluble plumbago alkene electrically conducting coating: the drying temperature of described coating is 50 ~ 100 DEG C, and time of drying is 30S ~ 10min.
Above-mentioned high-performance water-based graphene conductive coating can adopt spraying, spray ink Printing and typography in macromolecular material, metallic substance, ceramic surface preparation coating, the drying temperature of coating is 20 ~ 100 DEG C, time of drying is 30S ~ 10min, and obtained Graphene coating can be applicable to the fields such as electromagnetic shielding, antistatic, anticorrosion, heat radiation, wear-resisting and electronic circuit.
Embodiment
Below in conjunction with specific embodiment, the present invention is further illustrated.
Embodiment 1
Under condition of ice bath, 3.0g graphite is joined in the vitriol oil of 60ml, violent stirring 30min, further by 12gKMnO
4join in above-mentioned mixed solution, violent stirring 30min.Above-mentioned mixed solution is transferred in 30 DEG C of water-baths, slowly add 18gNaNO
3, stir 60min; Under agitation, 140ml deionized water is joined continuously in above-mentioned mixed solution, then transferred in the oil bath of 90 DEG C of temperature, stir the 30min time; Dropwise add 18mlH again
2o
2, continue reaction 60min and make solution become glassy yellow from dark-brown;
Under agitation, the dispersing agent PVP that consumption is the 1.5wt% of graphene oxide is added in above-mentioned graphene oxide solution, the hydrazine hydrate solution of 20ml is dripped after dissolving, 1h is reacted at 60 DEG C of temperature, 20ml20wt% acetic acid aqueous solution is dripped further in above-mentioned solution, continue reaction 30min, obtain stable graphene aqueous solution.In the aqueous solution of aforementioned stable, add 11wt% water polyacrylic acid, 0.15wt% thanomin, 0.15wt% monobutyl ether, 0.07wt% defoamer 901 successively, and be incorporated as the 1.5wt% melamino-formaldehyde of waterborne polyester.At temperature is 20 DEG C, stirs 30min, high-performance water-based graphene conductive coating can be obtained.The drying temperature of coating is 80 DEG C, and time of drying is 10min.
Embodiment 2
Under condition of ice bath, 3.0g graphite is joined in the vitriol oil of 60ml, violent stirring 30min, further by 12gKMnO
4join in above-mentioned mixed solution, violent stirring 30min.Above-mentioned mixed solution is transferred in 30 DEG C of water-baths, slowly add 18gNaNO
3, stir 60min; Under agitation, 140ml deionized water is joined continuously in above-mentioned mixed solution, then transferred in the oil bath of 90 DEG C of temperature, stir the 30min time; Dropwise add 18mlH again
2o
2, continue reaction 60min and make solution become glassy yellow from dark-brown;
Under agitation, the dispersing agent PVA that consumption is the 2.5wt% of graphene oxide is added in above-mentioned graphene oxide solution, the hydrazine hydrate solution of 20ml is dripped after dissolving, 1h is reacted at 80 DEG C of temperature, 20ml10wt% acetic acid aqueous solution is dripped further in above-mentioned solution, continue reaction 40min, obtain stable graphene aqueous solution.In the aqueous solution of aforementioned stable, add 11wt% water polyacrylic acid, 0.15wt% thanomin, 0.15wt% monobutyl ether, 0.07wt% defoamer 901 successively, and be incorporated as 2.5wt% melamino-formaldehyde, the 0.5wt% quadrol of waterborne polyester.At temperature is 20 DEG C, stirs 30min, high-performance water-based graphene conductive coating can be obtained.The drying temperature of coating is 50 DEG C, and time of drying is 4min.
Embodiment 3
Under condition of ice bath, 3.0g graphite is joined in the vitriol oil of 60ml, violent stirring 30min, further by 12gKMnO
4join in above-mentioned mixed solution, violent stirring 30min.Above-mentioned mixed solution is transferred in 30 DEG C of water-baths, slowly add 18gNaNO
3, stir 60min; Under agitation, 140ml deionized water is joined continuously in above-mentioned mixed solution, then transferred in the oil bath of 90 DEG C of temperature, stir the 30min time; Dropwise add 18mlH again
2o
2, continue reaction 60min and make solution become glassy yellow from dark-brown;
Under agitation, the dispersing agent PEG that consumption is the 2.5wt% of graphene oxide is added in above-mentioned graphene oxide solution, the hydrazine hydrate solution of 20ml is dripped after dissolving, 1h is reacted at 80 DEG C of temperature, 20ml15wt% acetic acid aqueous solution is dripped further in above-mentioned solution, continue reaction 50min, obtain stable graphene aqueous solution.In the aqueous solution of aforementioned stable, add 15wt% water polyacrylic acid, 0.35wt% thanomin, 0.25wt% monobutyl ether, 0.07wt% defoamer 901 successively, and be incorporated as 1.5wt% melamino-formaldehyde, the 1.5wt% quadrol of waterborne polyester.At temperature is 20 DEG C, stirs 30min, high-performance water-based graphene conductive coating can be obtained.The drying temperature of coating is 50 DEG C, and time of drying is 2min.
Embodiment 4
Under condition of ice bath, 3.0g graphite is joined in the vitriol oil of 60ml, violent stirring 30min, further by 12gKMnO
4join in above-mentioned mixed solution, violent stirring 30min.Above-mentioned mixed solution is transferred in 30 DEG C of water-baths, slowly add 18gNaNO
3, stir 60min; Under agitation, 140ml deionized water is joined continuously in above-mentioned mixed solution, then transferred in the oil bath of 90 DEG C of temperature, stir the 30min time; Dropwise add 18mlH again
2o
2, continue reaction 60min and make solution become glassy yellow from dark-brown;
Under agitation, the dispersing agent PEDOT:PSS that consumption is the 4.5wt% of graphene oxide is added in above-mentioned graphene oxide solution, the hydrazine hydrate solution of 20ml is dripped after dissolving, 1h is reacted at 70 DEG C of temperature, 20ml10wt% acetic acid aqueous solution is dripped further in above-mentioned solution, continue reaction 40min, obtain stable graphene aqueous solution.In the aqueous solution of aforementioned stable, add 11wt% water polyacrylic acid, 0.15wt% thanomin, 0.15wt% monobutyl ether, 0.07wt% defoamer 901 successively, and be incorporated as 2.5wt% melamino-formaldehyde, the 1.5wt% quadrol of waterborne polyester.At temperature is 20 DEG C, stirs 30min, high-performance water-based graphene conductive coating can be obtained.The drying temperature of coating is 70 DEG C, and time of drying is 50S.
Embodiment 5
Under condition of ice bath, 3.0g graphite is joined in the vitriol oil of 60ml, violent stirring 30min, further by 12gKMnO
4join in above-mentioned mixed solution, violent stirring 30min.Above-mentioned mixed solution is transferred in 30 DEG C of water-baths, slowly add 18gNaNO
3, stir 60min; Under agitation, 140ml deionized water is joined continuously in above-mentioned mixed solution, then transferred in the oil bath of 90 DEG C of temperature, stir the 30min time; Dropwise add 18mlH again
2o
2, continue reaction 60min and make solution become glassy yellow from dark-brown;
Under agitation, the dispersing agent PVP that consumption is the 4.5wt% of graphene oxide is added in above-mentioned graphene oxide solution, the hydrazine hydrate solution of 20ml is dripped after dissolving, 1h is reacted at 40 DEG C of temperature, 20ml40wt% hydriodic acid aqueous solution is dripped further in above-mentioned solution, continue reaction 40min, obtain stable graphene aqueous solution.In the aqueous solution of aforementioned stable, be incorporated as 17wt% water polyacrylic acid, 0.35wt% thanomin, 0.25wt% monobutyl ether, the 0.05wt% defoamer 902 of coating composition successively, and be incorporated as 2.5wt% melamino-formaldehyde, the 1.5wt% quadrol of waterborne polyester.At temperature is 20 DEG C, stirs 30min, high-performance water-based graphene conductive coating can be obtained.The drying temperature of coating is 80 DEG C, and time of drying is 30S.
Table 1. coating is prepared into conduction and the mechanical property of coating
Claims (10)
1. a preparation method for high-performance water-based graphene conductive coating, it is characterized in that, step is as follows:
(1) under condition of ice bath, 0.5 ~ 5.0g graphite is joined in the vitriol oil of 40ml ~ 60ml, violent stirring 30min; Further by 12 ~ 30g KMnO
4join in above-mentioned mixed solution, violent stirring 30min; Above-mentioned mixed solution is transferred in 30 DEG C of water-baths, slowly add 18 ~ 40gNaNO
3, stir 60min; Under agitation, 100 ~ 140ml deionized water is joined continuously in above-mentioned mixed solution, then transferred in the oil bath of 90 DEG C of temperature, stir the 30min time; Dropwise add 12 ~ 20mlH again
2o
2, continue reaction 40min ~ 80min until solution becomes glassy yellow from dark-brown;
(2) under agitation, in above-mentioned glassy yellow graphene oxide solution, add a certain amount of dispersing agent, drip the hydrazine hydrate solution of 15 ~ 45ml after dissolving, at 40 DEG C ~ 80 DEG C temperature, react 1h; In above-mentioned solution, drip 15 ~ 45ml also original reagent further, continue reaction 20 ~ 60min, obtain stable graphene aqueous solution;
(3) in the graphene aqueous solution of aforementioned stable, a certain amount of waterborne polyester, neutralizing agent, flow agent, defoamer, linking agent, catalytic reagent is added successively, stir certain hour at a certain temperature, high-performance water-based graphene conductive coating can be obtained.
2. the preparation method of watersoluble plumbago alkene electrically conducting coating as claimed in claim 1, it is characterized in that, in step (2), dispersing agent is PVP, PVA, PEG or PEDOT:PSS; The concentration of aqueous solution of dispersing agent is 0.5 ~ 20wt%.
3. the preparation method of watersoluble plumbago alkene electrically conducting coating as claimed in claim 1, it is characterized in that, in step (2), going back original reagent is acetic acid or hydroiodic acid HI; Acetic acid aqueous solution concentration is 10 ~ 30wt%, and hydriodic acid aqueous solution concentration is 10 ~ 40wt%.
4. the preparation method of watersoluble plumbago alkene electrically conducting coating as claimed in claim 1, it is characterized in that, in step (3), described neutralizing agent is ethanolamines, and flow agent is only son's ethers, and defoamer is defoamer 901 or 902.
5. the preparation method of the watersoluble plumbago alkene electrically conducting coating as described in claim 1 or 4, it is characterized in that, described waterborne polyester, neutralizing agent, flow agent, defoamer consumption are respectively 5 ~ 20wt%, 0.1 ~ 2wt%, 0.15 ~ 0.5wt%, the 0.02 ~ 0.1wt% of coating composition.
6. the preparation method of watersoluble plumbago alkene electrically conducting coating as claimed in claim 1, it is characterized in that, described linking agent is melamino-formaldehyde or aminoresin class, and add-on is 5 ~ 25wt% of waterborne polyester.
7. the preparation method of watersoluble plumbago alkene electrically conducting coating as claimed in claim 1, it is characterized in that, described catalytic reagent is ethylenediamines, and add-on is 0 ~ 2.0wt% of waterborne polyester.
8. the preparation method of watersoluble plumbago alkene electrically conducting coating as claimed in claim 1, it is characterized in that, described coating whipping temp is 5 ~ 30 DEG C, and churning time is 10min ~ 3 hour.
9. adopt the watersoluble plumbago alkene electrically conducting coating that described in any one of claim 1 to 8, method prepares.
10. the purposes of watersoluble plumbago alkene electrically conducting coating prepared of method described in any one of claim 1 to 8, it is characterized in that, this coating is used for spraying, spray ink Printing and typography and prepares coating; This coating be used in macromolecular material, metallic substance, ceramic surface, for electromagnetic shielding, antistatic, anticorrosion, heat radiation, wear-resisting and field of electronic circuitry.
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