CN109777214A - Graphene static conductive priming paint and preparation method thereof - Google Patents
Graphene static conductive priming paint and preparation method thereof Download PDFInfo
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- CN109777214A CN109777214A CN201711126820.5A CN201711126820A CN109777214A CN 109777214 A CN109777214 A CN 109777214A CN 201711126820 A CN201711126820 A CN 201711126820A CN 109777214 A CN109777214 A CN 109777214A
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Abstract
The present invention provides a kind of graphene static conductive priming paint and preparation method thereof.The priming paint includes each component of following mass parts: 0.01-0.8 parts of 35-55 parts of film forming matter, graphene or graphene complex, 8-42 parts of complex conductive filler, 8-42 parts of titanium dioxide, dispersing agent I are 0.005-1.6 parts, dispersing agent II is 1.5-5 parts, 0.5-3 parts of auxiliary agent, 5-20 parts of solvent.For the lightness (L value) of the priming paint more than 60, resistance is lower than 0.1M Ω.
Description
Technical field
The invention belongs to field of nanocomposite materials, are related to a kind of priming paint containing graphene, and in particular to a kind of graphite
Alkene static conductive priming paint and preparation method thereof.
Background technique
Static conductive coating is that will there are the pigments and fillers of conducting function to be added in resin matrix, assigns composite coating transmission electricity
The function of lotus.Conductive filler is the critical material of various static conductive coatings.Mainly there is carbon black using more conductive filler at present
With metal powder (silver, copper, nickel), complex conductive filler (Conductive mica, conductive titanium dioxide, conductive silica flour) etc..Metal powder
End is expensive, is oxidized easily, and additive amount is big when use, is easy sedimentation, and color is deeper.Carbon black price is lower, still
It is added in priming paint, coating color can be made deeper, not easy-regulating, and is difficult to disperse.Therefore, it is dedicated to developing both at home and abroad compound
Conductive filler, complex conductive filler are so that mica, titanium dioxide, silica flour is had electric conductivity by metal-doped modification.Mesh
Before, conductive titanium dioxide is the complex conductive filler being most widely used, however, traditional conductive titanium dioxide is in practical applications
Degradation rate is higher, cannot be properly arrived at the requirement of permanent conductive, antistatic.
As people's awareness of environmental protection continues to increase, highly energy-consuming, low-energy-efficiency conventional air spraying process be gradually eliminated,
Novel spraying technique and facility obtain continuous promotion and application.Electrostatic spraying overcomes conventional air and sprays seriously polluted, painting
Expect utilization rate it is low, to comprehensive coating of complex part there are apparent dead angle, secondary cleaning cost is higher the disadvantages of, have simultaneously
Coating quality is good, operating environment is good, saves the advantages that coating, greatly promotes painting rate and production efficiency, comprehensive benefit is very
Obviously.Currently, the static conductive priming paint for electrostatic spraying is mainly by compounding carbon black with titanium dioxide, or add compound
Conductive filler meets the conduction needs of priming paint.And conductive titanium dioxide cannot be ground, and largely when addition, be not able to satisfy for thin
Spend the demand of more demanding coating.
Chinese invention patent CN103923552B discloses a kind of " High-performance graphene-acicular titanium dioxide conductive coating
And preparation method thereof ", which, using aqueous epoxy resin emulsion as matrix, is to lead with graphene-acicular titanium dioxide dispersion liquid
Needle-like conductive titanium dioxide, is add to deionized water to form the slurry that solid content is 5~20% first by electric filler, and heating is stirred
It mixes to 40~90 DEG C, then according to " mass ratio of acicular titanium dioxide and graphene be added for 0.5:1~2:1 graphene ", after
Continuous ultrasonic disperse 1~5 hour, prepares graphene-acicular titanium dioxide dispersion liquid, then by the dispersion liquid and aqueous epoxy resins
Lotion and the mixing of other coating additives are uniformly dispersed obtained conductive coating, and in this method, graphene is in the needle-shaped titanium dioxide of graphene-
Mass fraction in titanium dispersion liquid is big, is not easy ultrasonic disperse.In the presence of surfactant-free, dispersion of the graphene in aqueous solution
In the process, due to the effect of graphene high specific surface area and Van der Waals force itself, easily reunite and stack again.Middle promulgated by the State Council
Bright patent CN106009984A discloses " a kind of graphene/acrylic acid static conductive coating and preparation method thereof ", stone in the patent
The mass ratio of black alkene and dispersing agent is (1-20): 1, the mass ratio of graphene and acrylic resin is 1:(20-1000), then add
The graphene/acrylic acid static conductive coating is prepared in other auxiliary agents, and the surface resistivity for measuring the coating is 1M Ω, still
The static conductive coating that the patent is discussed does not investigate the color demand of coating, according to document and the long-term reality of this patent author
It tests, it is found that the priming paint appearance under patent proportion is black, be not suitable for the field more demanding for Color whiteness.
Currently, developing the high static conductive priming paint of good conductivity, lightness is the major issue that domestic and international material circle is paid close attention to for a long time
One of, related work still needs to reinforce.In view of this, special propose the invention.
The content of background technology part is only the technology that inventor is known, not the existing skill of natural representative this field
Art.
Summary of the invention
The first object of the present invention is to realize graphene or graphene complex and conductive titanium dioxide by simple technique
It is uniform compound, obtain the electrically conductive composite of function admirable.
Claimed priming paint, each component including following mass parts: 35-55 parts of film forming matter, graphene or
0.01-0.8 parts of graphene complex, 8-42 parts of complex conductive filler, 8-42 parts of titanium dioxide, dispersing agent I are 0.005-1.6
Part, dispersing agent II are 1.5-5 parts, 0.5-3 parts of auxiliary agent, 5-20 parts of solvent.
In above-mentioned priming paint, the mass parts of each component concretely:
Concretely 35,40,41,42,45.2,46,47,48,50 or 52.45 parts of the film forming matter；
The graphene or graphene complex concretely 0.01,0.05,0.08,0.2,0.4,0.6,0.65,0.8
Part；
Concretely 8,9,10,17,20,35,36,30,32.62,36 parts of the complex conductive filler；
Concretely 8,10,12,14,16.5,17,18,20,23,25,26,34,35,40 or 42 parts of the titanium dioxide；
Concretely 0.02,0.05,0.1,0.2,0.4,0.6,1.0,1.2,1.4 or 1.6 part of the dispersing agent I；
Concretely 1.5,1.6,1.7,1.8,2,2.4,2.9,3,3.2,4 or 4.5 parts of the dispersing agent II；
Concretely 0.5,0.8,1,1.2,1.5,1.6,1.8,2.5,2.77,2.8 or 3 part of the auxiliary agent；
Concretely 5,6,7,10,14.5,15 or 20 parts of the solvent；
Specifically, the claimed priming paint of aforementioned present invention may include each component of following mass parts: film forming matter 40-50
Part, graphene or 0.1-0.5 parts of graphene complex, 10-35 parts of complex conductive filler, 10-35 parts of titanium dioxide, dispersing agent I
For 0.05-1 parts, II 2-4 parts of dispersing agent, 1-2.5 parts of auxiliary agent, 5-15 parts of solvent；
More specifically, the priming paint includes each component of following mass parts: 45-50 parts of film forming matter, graphene or graphite
0.05-0.2 parts of alkene compound, 25-35 parts of complex conductive filler, 12-25 parts of titanium dioxide, dispersing agent are I 0.02-0.2 parts, divide
II 2.4-5 parts of powder, 1.5-3 parts of auxiliary agent, 15-20 parts of solvent；
Again specifically, the priming paint includes each component of following mass parts: 44.6 parts of film forming matter, graphene or graphene
0.2 part of compound, 25 parts of complex conductive filler, 25 parts of titanium dioxide, dispersing agent I are 0.2 part, dispersing agent II is 3 parts, auxiliary agent 2
Part, 14.5 parts of solvent.
In above-mentioned priming paint, the film forming matter is selected from acrylic resin, epoxy resin, fluorocarbon resin and superchlorinated polyvinyl chloride resin
At least one of；
The graphene complex is the composite material by graphene and other carbon materials, other described carbon materials include carbon
Nanotube and/or conductive black；
The complex conductive filler is conductive titanium dioxide, conductive mica powder or conductive silica flour；The compound-type conducting
Filler is preferably conductive titanium dioxide；
The titanium dioxide is anatase thpe white powder；
The dispersing agent I is anionic, cationic, amphoteric or high-molecular type dispersing agent；
The dispersing agent II is high-molecular type dispersing agent；
The auxiliary agent is selected from least one of anti-settling agent, levelling agent and defoaming agent；The solvent is selected from toluene, diformazan
Benzene, ethyl acetate, butyl acetate, N,N-dimethylformamide, DMAC N,N' dimethyl acetamide, dehydrated alcohol, isopropanol and adjacent benzene
At least one of dibutyl carboxylic acid.
In the film forming matter, the acrylic resin is the thermoplastic acrylic that weight average molecular weight is 80000-90000
Resin；
The epoxy resin is the epoxy resin of low epoxide number < 0.5；
The fluorocarbon resin is the thermoplastic fluorocarbon resin that weight average molecular weight is 20000-50000；
The superchlorinated polyvinyl chloride resin is middle low viscosity superchlorinated polyvinyl chloride resin；
In the graphene complex, the mass fraction of graphene is 10%-90%；Concretely 33%, 50%,
90%, 30%-90%, 30%-60%, 40%-60% or 60%-90%；
Specifically, the method for preparing the graphene complex, comprising: lead to graphene and carbon nanotube or conductive black
It crosses blending and/or modified technique is combined；
More specifically, the method for the graphene complex is prepared, comprising: be added after mixing modifying agent with stirring solvent
Graphene and carbon nanotube or conductive black, are stirred to react and finish to obtain the final product；
Again specifically, in the modifying agent and stirring solvent mixing, speed of agitator 500-1000rpm；Mixing time is
10-30min；Whipping temp is 50-100 DEG C, concretely 80 DEG C；Graphene and carbon nanotube or the conductive black of being added
It is stirred to react in step, speed of agitator 2000-3000rpm；Reaction time is 0.5-2h, concretely 1h；Reaction temperature is
50-100 DEG C, concretely 80 DEG C；
The modifying agent is chosen in particular from least one of octadecylamine, dodecyl benzene sulfonic acid and oleic acid；
The solvent is chosen in particular from least one in dimethylbenzene, ethyl acetate, N,N-dimethylformamide and dehydrated alcohol
Kind；
The dosage of the modifying agent is specially the 10%-20% of the gross mass of the graphene and carbon nanotube or carbon black；
Concretely 13.3%；
In the dispersing agent I, anionic dispersing agent I is in carboxylate, sulfuric ester, phosphate ester salt and sulfonate type
It is at least one；
Cationic dispersing agent I is selected from least one of alkyl quaternary ammonium salts, amino propylamine dioleate and quaternary ammonium salt；
Amphoteric dispersing agent I is carboxylate；
High-molecular type dispersing agent I is selected from least one of natural polymer dispersing agent and synthesis macromolecule dispersing agent；
The dispersing agent I be chosen in particular from BYK163, BYK161, BYK110, BYK118, Disponer 9850,
SOLSPERSE37500、SOLSPERSE V350、SOLSPERSE20000、SOLSPERSE44000、S-601、Silok-7423、
Dispers 610S、S-4010B、DA-01、DA-168、DA-1040、Tech 6320、Tech-510、DA-703-50、
In WinSperse4900, WinSperse3030, WinSperse3050, WinSperse3300 and WinSperse3204 extremely
Few one kind；
The dispersing agent II be chosen in particular from BYK163, BYK161, BYK110, DA-P10, DA-01, DA-168, DA-1040,
Tech-510、Disperbyk-180、WinSperse3030、WinSperse3050、WinSperse3300、
WinSperse3204, Dispex Ultra FA 4420, ZetaSperse 370, Sokalan CP 9, Ecodis P90 and
At least one of Tego Dispers 740W；
The anti-settling agent is N-Methyl pyrrolidone solution, the modified hydrogenated castor oil, titanate coupling agent of modified polyurea
Or polyamide wax；It is preferred that the N-Methyl pyrrolidone solution of modified polyurea；
The relative molecular mass of the polyamide wax is specially 1500-3000；
The anti-settling agent be chosen in particular from BYK-410, BYK-411, BYK-7411ES, FC-100, A630-SV, YB-301,
At least one of EFKA 3777N, DAPRO BEZ 75, NDZ-201 and GHDY920-20X；
The levelling agent is organic silicon type levelling agent or esters of acrylic acid levelling agent；
The levelling agent is chosen in particular from BYK-323, BYK-352, BYK-354, BYK-333, BYK-3550, Silok-
8358, at least one of Silok-8488 and EFKA 3777N；
The defoaming agent is non-silicon class defoaming agent, polyethers defoaming agent or phosphoric acid ester defoaming agent；
The defoaming agent is chosen in particular from BYK-017, BYK-018, BYK-051N, BYK-052N, BYK-1752, BYK-
8821、B-224、B-225、Foamaster MO 2190AC、Tego Foamex 3062、XIAMETER AFE-1430、
At least one of Silok-4082, Silok-4084 and Silok-4075；
The mass ratio of the anti-settling agent, levelling agent and defoaming agent is 1.3-20:1:1-4；It is preferred that 2:1:1.
In the priming paint, the graphene or graphene complex, complex conductive filler and the graphene or graphite
Piece-point-chip architecture conductive network that alkene compound is formed；Wherein, the complex conductive filler is inserted into the graphene
Or in the lamella of graphene complex；
The L value (lightness) of the priming paint is greater than 60；And/or
The resistance of the priming paint is lower than 0.1M Ω.
The second object of the present invention is to provide a kind of preparation method of graphene static conductive priming paint.Priming paint prepared by the present invention
Electric conductivity and good mechanical property, lightness it is high, and the priming paint prepared by this patent the method, the interface of priming paint and matrix
It is combined, the long service life of priming paint, there is good application value.
The preparation method of claimed priming paint, using the group of proportional quantity in aforementioned priming paint provided by the invention
Point, comprising:
It is first that part film forming matter is uniform with stirring solvent, sequentially add dispersing agent I and the graphene or graphene
Compound, grinding；
Part dispersing agent II and complex conductive filler are added, is stirred and evenly mixed, components I is obtained；
Remaining film forming matter, remaining dispersing agent II and titanium dioxide are stirred and evenly mixed, then mixture is ground, obtains group
Divide II；With
By the components I, the compositionⅱ and auxiliary agent be uniformly mixed to get.
In the above method, the part film forming matter is the 30wt%-75wt% of film forming matter；Concretely 40wt%,
49wt%, 53wt%, 59wt%, 60wt%, 62wt% or 65wt%；It is preferred that 50wt%；
The part dispersing agent II is the 20-75wt% of dispersing agent II；Concretely 33wt%, 37.5wt%, 56wt%,
62.5wt%, 68wt%, 69wt% or 75wt%；It is preferred that 50wt%.
In the part film forming matter and stirring solvent homogenizing step, mixing time 10-20min, speed of agitator is
400-1200rpm, concretely 500rpm, 600rpm, 900rpm or 1100rpm；Preferably, mixing time 15min, stirring
Revolving speed is 1000rpm；
In the grinding steps that dispersing agent I and the graphene or graphene complex is added, it is ground to mixed material
Fineness less than 10 microns；Preferably, milling time 2-5h, concretely 2.5h, 3.5h or 4h；Grinding revolving speed is
1500rpm-3500rpm, concretely 2300rpm, 2500rpm, 2800rpm or 3000rpm；Preferably, milling time 3h,
Grinding revolving speed is 2000rpm.
It is described be added after part dispersing agent II and complex conductive filler the step of stirring and evenly mixing in, mixing time is
20min-60min, concretely 30min, 35min, 40min, 45min or 50min；Speed of agitator is 1000rpm-2000rpm,
Concretely 1400rpm, 1600rpm or 1800rpm；Preferably, mixing time 30min, speed of agitator 1500rpm.
In described the step of stirring and evenly mixing remaining film forming matter, remaining dispersing agent II and titanium dioxide, mixing time
For 10-20min, concretely 16min；Speed of agitator 200-1000rpm, concretely 300rpm or 500rpm；Preferably, it stirs
Mixing the time is 15min；Speed of agitator is 800rpm；
It is described remaining film forming matter, remaining dispersing agent II and titanium dioxide are stirred and evenly mixed after grinding steps in, grind
II fineness of obtained component is milled to less than 25 microns；Preferably, milling time 0.5-2h, concretely 1.5h；Grinding revolving speed is
1500rpm-3500rpm, concretely 1600rpm, 2500rpm or 3000rpm；It is further preferred that milling time is 1h；It grinds
Mill revolving speed is 2000rpm.
The third object of the present invention is that aforementioned priming paint provided by the invention is claimed to prepare answering in static conductive priming paint
With and containing aforementioned priming paint provided by the invention static conductive priming paint.
The present invention provides a kind of graphene static conductive priming paint and its preparation for defect existing in terms of static conductive priming paint
Method.For the lightness (L value) of the priming paint more than 60, resistance is lower than 0.1M Ω.
Detailed description of the invention
Attached drawing is used to provide further understanding of the present invention, and constitutes part of specification, with reality of the invention
It applies example to be used to explain the present invention together, not be construed as limiting the invention.In the accompanying drawings:
Fig. 1 is according to Chinese invention patent CN106009984A " a kind of graphene/acrylic acid static conductive coating and its preparation
Method " in embodiment 3 prepare coating；
Fig. 2 is the coating that the embodiment of the present invention 10 is prepared.
Specific embodiment
The present invention is further elaborated combined with specific embodiments below, but the present invention is not limited to following embodiments.Institute
State method is conventional method unless otherwise instructed.The raw material can obtain unless otherwise instructed from public commercial source.
Acrylic resin used in following embodiments is purchased from Changzhou City Bohe Paint Co., Ltd, and product number is
BHR822 is the thermoplastic acrylic resin that weight average molecular weight is 80000-90000；Epoxy resin used is purchased from commonly
E44 type epoxy resin, low epoxide number < 0.5；Superchlorinated polyvinyl chloride resin used is middle low viscosity superchlorinated polyvinyl chloride resin, is purchased from Weifang
Gao Xin Chemical Industry Science Co., Ltd, product number HCPE-L；Fluorocarbon resin used is purchased from Changshu three and likes that Fu Zhonghao chemical industry is new
Materials Co., Ltd, product number are JF-2X (admittedly containing 50%), are the thermoplastic fluoroelastomer carbon that weight average molecular weight is 20000-50000
Resin.Titanium dioxide used is purchased from Du Pont, model R901.Conductive titanium dioxide used is purchased from preceding Hai Jishengya (Shenzhen) science and technology
Co., Ltd, model MTI-02；Conductive mica powder used is purchased from Shanghai De Yu get trade Co., Ltd, model TS-
210；Conduction silica flour used is purchased from Xuzhou Jinya Powder Co., Ltd..
Embodiment 1:
(1) acrylic resin (admittedly containing 46.5%) 61.9g, dimethylbenzene 5g, toluene 5g, mechanical stirring 10min are weighed,
Then 0.005g dispersing agent Tech 6320,0.01g graphene is added in 600rpm, grind 2h, and revolving speed 2500rpm is ground to
The fineness of mixed material is 8-10 microns, and component A is obtained after filtering.
(2) 1.0g dispersant B YK161,36g conductive titanium dioxide is added in Xiang Shangshu component A, stirs 30min, 1800rpm,
Obtain components I.
(3) acrylic resin (admittedly containing 46.5%) 41.29g is weighed, 0.5g dispersant B YK161,14g titanium dioxide machine are added
Tool stirs 10min, revolving speed 1000rpm, and the mixture is then ground 1.5h again, and revolving speed 2000rpm is ground to fineness less than 25
Micron, obtains compositionⅱ after filtering.
(4) components I, compositionⅱ and 0.3g anti-settling agent BYK-411,0.1g levelling agent Silok-8358,0.1g are defoamed
Agent BYK-017 is uniformly mixed, and obtains graphene static conductive priming paint 1.
Embodiment 2:
(1) acrylic resin (admittedly containing 46.5%) 75.3g, dimethylbenzene 2g, butyl acetate 4g, mechanical stirring 15min are weighed,
Then 0.15g dispersing agent WinSperse3204,0.05g graphene is added in 900rpm, grind 3.5h, and revolving speed 2300rpm is ground
The fineness for being milled to mixed material is 7-9 microns, and component A is obtained after filtering.
(2) 1.5g dispersant B YK163,25g conductive titanium dioxide is added in Xiang Shangshu component A, stirs 40min, 1000rpm,
Obtain components I.
(3) acrylic resin (admittedly containing 46.5%) 32.3g is weighed, addition 0.5g dispersant B YK163,17g titanium dioxide is mechanical
16min, revolving speed 800rpm are stirred, the mixture is then ground into 2h, revolving speed 1600rpm again, is ground to fineness less than 25 microns,
Obtain compositionⅱ.
(4) by components I, compositionⅱ and 0.4g anti-settling agent BYK-410,0.2g levelling agent BYK-333,0.2g defoaming agent
BYK-052N is uniformly mixed, and obtains graphene static conductive priming paint 2.
Embodiment 3:
(1) acrylic resin (admittedly containing 46.5%) 64.13g, butyl acetate 5g, toluene 2g, mechanical stirring 20min are weighed,
Then I WinSperse3300,0.1g graphene of 0.4g high-molecular type dispersing agent is added in 500rpm, grind 2.5h, and revolving speed is
2800rpm, the fineness for being ground to mixed material is 7-9 microns, and component A is obtained after filtering.
(2) 1.0g dispersant B YK110,26g conductive titanium dioxide is added in Xiang Shangshu component A, stirs 40min, 1400rpm,
Obtain components I.
(3) acrylic resin (admittedly containing 46.5%) 42.75g is weighed, 0.8g dispersant B YK110,23g titanium dioxide machine are added
Tool stirs 10min, revolving speed 800rpm, and the mixture is then ground 1.5h again, and revolving speed 2500rpm is ground to fineness less than 25
Micron, obtains compositionⅱ after filtering.
(4) by components I, compositionⅱ (48 parts) and 0.5g anti-settling agent FC-100,0.25g levelling agent Silok-8358,
0.25g defoaming agent Silok-4082 is uniformly mixed, and obtains graphene static conductive priming paint 3.
Embodiment 4:
(1) acrylic resin (admittedly containing 46.5%) 42.75g, dimethylbenzene 3g is weighed, n,N-Dimethylformamide 2g is mechanical
15min, 1100rpm are stirred, 1.0g dispersing agent WinSperse4900,0.4g graphene is then added, grinds 4h, revolving speed is
3000rpm, the fineness for being ground to mixed material is 8-9 microns, and component A is obtained after filtering.
(2) 0.8g dispersing agent DA-01,20g conductive titanium dioxide is added in Xiang Shangshu component A, stirs 45min, 1500rpm,
Obtain components I.
(3) acrylic resin (admittedly containing 46.5%) 64.13g is weighed, addition 0.9g dispersing agent DA-01,26g titanium dioxide is mechanical
20min, revolving speed 800rpm are stirred, the mixture is then ground into 1h, revolving speed 3000rpm again, is ground to fineness less than 25 microns,
Compositionⅱ is obtained after filtering.
(4) components I, compositionⅱ and 0.8g anti-settling agent BYK-7411ES, 0.2g levelling agent BYK-3550,0.2g are defoamed
Agent Tego Foamex 3062 is uniformly mixed, and obtains graphene static conductive priming paint 4.
Embodiment 5:
(1) acrylic resin (admittedly containing 46.5%) 48.6g, dimethylbenzene 2g, ethyl acetate 1g, dehydrated alcohol 2g, machine are weighed
Tool stirs 15min, 1200rpm, and 1.2g dispersing agent SOLSPERSE20000,0.5g graphene is then added, and grinds 3h, and revolving speed is
3500rpm, the fineness for being ground to mixed material is 8-10 microns, and component A is obtained after filtering.
(2) 1.0g dispersing agent WinSperse3030,17g conductive titanium dioxide is added in Xiang Shangshu component A, stirs 35min,
1600rpm obtains components I.
(3) acrylic resin (admittedly containing 46.5%) 42.6g is weighed, 0.6g dispersing agent WinSperse3030,34g titanium is added
White powder mechanical stirring 20min, revolving speed 800rpm, then grind 1.5h for the mixture again, and revolving speed 2500rpm is ground to fineness
Less than 25 microns, compositionⅱ is obtained after filtering.
(4) by components I, compositionⅱ and 1g anti-settling agent NDZ-201,0.2g levelling agent Silok-8488,0.4g defoaming agent
BYK-1752, it is uniformly mixed, obtains graphene static conductive priming paint 5.
Embodiment 6:
(1) acrylic resin (admittedly containing 46.5%) 60g, dimethylbenzene 2g, n,N-dimethylacetamide 3g, mechanical stirring are weighed
Then 0.6g dispersing agent S-4010B, 0.6g graphene is added in 15min, 1000rpm, grind 3.5h, and revolving speed 3000rpm is ground
The fineness for being milled to mixed material is 9-10 microns, and component A is obtained after filtering.
(2) 1.5g dispersing agent Tech-510,10g conductive titanium dioxide is added in Xiang Shangshu component A, stirs 20min,
1000rpm obtains components I.
(3) acrylic resin (admittedly containing 46.5%) 41.72g is weighed, 2.5g dispersing agent Tech-510,35g titanium dioxide is added
Mechanical stirring 15min, revolving speed 800rpm, then grind 2h for the mixture again, and revolving speed 2500rpm is ground to fineness less than 25
Micron, obtains compositionⅱ after filtering.
(4) components I, compositionⅱ and 2g anti-settling agent EFKA 3777N, 0.1g levelling agent Silok-8488,0.4g are defoamed
Agent B-225 is uniformly mixed, and obtains graphene static conductive priming paint 6.
Embodiment 7:
(1) acrylic resin (admittedly containing 46.5%) 26.65g, dimethylbenzene 3g, isopropanol 3g, mechanical stirring 15min are weighed,
Then 1.6g dispersing agent Silok-7423,0.8g graphene is added in 1200rpm, grind 5h, and revolving speed 3500rpm is ground to mixed
The fineness for closing material is 7-10 microns, and component A is obtained after filtering.
(2) 1.5g dispersing agent DA-01,9g conductive titanium dioxide is added in Xiang Shangshu component A, is stirred 30min, 1000rpm, is obtained
To components I.
(3) acrylic resin (admittedly containing 46.5%) 62.17g is weighed, addition 3g dispersing agent DA-01,40g titanium dioxide machinery stirs
20min, revolving speed 1000rpm are mixed, the mixture is then ground into 2h, revolving speed 3500rpm again, is ground to fineness less than 25 microns,
Compositionⅱ is obtained after filtering.
(4) by components I, compositionⅱ and 2g anti-settling agent A630-SV, 0.3g levelling agent Silok-8488,0.5g defoaming agent
BYK-8821 is uniformly mixed, and obtains graphene static conductive priming paint 7.
Embodiment 8:
(1) acrylic resin (admittedly containing 46.5%) 45.91g, dimethylbenzene 10g, dibutyl phthalate 10g, machine are weighed
Tool stirs 20min, 400rpm, and 1.4g dispersant B YK118,0.65g graphene is then added, and grinds 3h, revolving speed 2500rpm,
The fineness for being ground to mixed material is 7-10 microns, and component A is obtained after filtering.
(2) 1.0g dispersing agent Tech-510,8g conductive titanium dioxide is added in Xiang Shangshu component A, stirs 20min,
2000rpm obtains components I.
(3) acrylic resin (admittedly containing 46.5%) 40g is weighed, addition 4g dispersing agent Tech-510,42g titanium dioxide machinery stirs
15min, revolving speed 1000rpm are mixed, the mixture is then ground into 1.5h again, it is micro- less than 25 to be ground to fineness by revolving speed 3000rpm
Rice, obtains compositionⅱ after filtering.
(4) by components I, compositionⅱ and 2g anti-settling agent A630-SV, 0.5g levelling agent BYK-333,0.5g defoaming agent
Foamaster MO 2190AC is uniformly mixed, and obtains graphene static conductive priming paint 8.
Embodiment 9:
(1) 0.1g octadecylamine is mixed with 50 milliliters of dehydrated alcohols, at 80 DEG C, 500rpm stirs 30min, and 0.9g stone is added
Black alkene and 0.1g carbon nanotube, 2000rpm is stirred to react 1h, after the completion of 80 DEG C of stirrings of temperature, washing, filtering, it is dry to get
To the compound of graphene and carbon nanotube.
(2) epoxy resin (admittedly containing 40%) 75g, dimethylbenzene 5g is weighed, then mechanical stirring 15min, 1000rpm are added
Graphene obtained by 0.1g dispersing agent WinSperse3030,0.15g step 1) and carbon mano-tube composite, grind 3h, and revolving speed is
2000rpm, the fineness for being ground to mixed material is 8-10 microns, and component A is obtained after filtering.
(3) 3.4g dispersant B YK161,30g conductive mica powder is added in Xiang Shangshu component A, stirs 30min, 1800rpm,
Obtain components I.
(4) epoxy resin (admittedly containing 40%) 40g is weighed, addition 1.6g dispersant B YK161,16.55g titanium dioxide machinery stirs
15min, revolving speed 800rpm are mixed, the mixture is then ground into 1h, revolving speed 2000rpm again, is ground to fineness less than 25 microns, mistake
Compositionⅱ is obtained after filter.
(5) by components I, compositionⅱ and 1.6g anti-settling agent BYK-410,0.2g levelling agent BYK-354,0.4g defoaming agent
BYK-8821 is uniformly mixed, and obtains graphene static conductive priming paint 9.
Embodiment 10:
(1) acrylic resin (admittedly containing 46.5%) 47.96g, dimethylbenzene 14.5g, mechanical stirring 15min are weighed,
Then 0.2g dispersing agent WinSperse3204,0.2g graphene is added in 1000rpm, grind 3h, revolving speed 2000rpm, grinding
Fineness to mixed material is 8-10 microns, obtains component A.
(2) 1.5g dispersant B YK161,25g conductive titanium dioxide is added in Xiang Shangshu component A, stirs 30min, 1500rpm,
Obtain components I.
(3) acrylic resin (admittedly containing 46.5%) 47.96g is weighed, 1.5g dispersant B YK161,25g titanium dioxide machine are added
Tool stirs 15min, revolving speed 800rpm, and the mixture is then ground 1h again, and it is micro- less than 25 to be ground to fineness by revolving speed 2000rpm
Rice, obtains compositionⅱ.
(4) by components I, compositionⅱ (48 parts) and 1g anti-settling agent BYK-410,0.5g levelling agent Silok-8488,0.5g
Defoaming agent Silok-4082 is uniformly mixed, and obtains graphene static conductive priming paint 10.
Embodiment 11:
(1) superchlorinated polyvinyl chloride resin (admittedly containing 50%) 60g, butyl acetate 10g, mechanical stirring 20min, 1000rpm are weighed, so
0.05g dispersing agent Tech-6320,0.05g graphene is added afterwards, grinds 4h, revolving speed 3000rpm is ground to mixed material
Fineness is 8-9 microns, and component A is obtained after filtering.
(2) 1.5g dispersant B YK161,35g conduction silica flour are added in Xiang Shangshu component A, stir 45min, 1500rpm,
Obtain components I.
(3) superchlorinated polyvinyl chloride resin (admittedly containing 50%) 38g is weighed, addition 0.9g dispersant B YK161,12g titanium dioxide machinery stirs
15min, revolving speed 1000rpm are mixed, the mixture is then ground into 2h again, revolving speed 2000rpm obtains compositionⅱ after filtering.
(4) by components I, compositionⅱ and 1g anti-settling agent BYK-411,0.25g levelling agent BYK-3550,0.25g defoaming agent
XIAMETER AFE-1430 is uniformly mixed, and obtains graphene static conductive priming paint 11.
Embodiment 12:
(1) 0.4g dodecyl benzene sulfonic acid is mixed with 100 milliliters of n,N-Dimethylformamide, at 60 DEG C, 1000rpm is stirred
10min is mixed, 1g graphene and 1g conductive black is added, 3000rpm is stirred to react 0.5h and washes after the completion of temperature 60 C stirring
It washs, filter, drying to get the compound of graphene and conductive black is arrived.
(2) fluorocarbon resin (admittedly containing 50%) 78.87g, dimethylbenzene 5g, mechanical stirring 10min, 1200rpm are weighed, then plus
Enter the compound of graphene and conductive black obtained by 0.1g dispersing agent WinSperse3300,0.08g step 1), grinds 3h, revolving speed
For 2000rpm, the fineness for being ground to mixed material is 9-10 microns, and component A is obtained after filtering.
(3) 2g dispersant B YK110,32.62g conductive titanium dioxide is added in Xiang Shangshu component A, stirs 50min,
1500rpm obtains components I.
(4) fluorocarbon resin (admittedly containing 50%) 26.29g is weighed, addition 0.9g dispersant B YK110,10g titanium dioxide machinery stirs
10min, revolving speed 300rpm are mixed, the mixture is then ground into 2h, revolving speed 2000rpm again, is ground to fineness less than 25 microns, mistake
Compositionⅱ is obtained after filter.
(5) by components I, compositionⅱ and 1g anti-settling agent YB-301,0.4g levelling agent Silok-8488,0.4g defoaming agent
BYK-051N is uniformly mixed, and obtains graphene static conductive priming paint 12.
Embodiment 13:
(1) 0.4g oleic acid is uniformly mixed with 100 milliliters of dehydrated alcohols, at 50 DEG C, 1000rpm stirs 10min, and 1g is added
Graphene and 0.5g conductive black, 0.5g carbon nanotube, 3000rpm is stirred to react 1h, after the completion of temperature 50 C stirring, washing,
Filtering is dried to get graphene complex is arrived.
(2) acrylic resin (admittedly containing 46.5%) 67.53g, dimethylbenzene 5g, mechanical stirring 15min, 1200rpm are weighed, so
Graphene complex obtained by 0.02g dispersing agent WinSperse4900,0.01g step 1) is added afterwards, grinds 2.5h, revolving speed is
2000rpm, the fineness for being ground to mixed material is 7-10 microns, and component A is obtained after filtering.
(3) 2g dispersant B YK163,26g conductive titanium dioxide is added in Xiang Shangshu component A, is stirred 30min, 1500rpm, is obtained
To components I.
(4) acrylic resin (admittedly containing 46.5%) 40g is weighed, addition 1.2g dispersant B YK163,18g titanium dioxide machinery stirs
10min, revolving speed 500rpm are mixed, the mixture is then ground into 1h, revolving speed 2000rpm again, is ground to fineness less than 25 microns, mistake
Compositionⅱ is obtained after filter.
(5) by components I, compositionⅱ and 1g anti-settling agent BYK-411,1g levelling agent EFKA 3777N, 1g defoaming agent BYK-
018 is uniformly mixed, and obtains graphene static conductive priming paint 13.
Embodiment 14:
(1) acrylic resin (admittedly containing 46.5%) 46.02g, dimethylbenzene 15g, mechanical stirring 15min, 1000rpm are weighed,
Then 1.6g dispersing agent S-601,0.4g graphene is added, grinds 3h, revolving speed 2000rpm is ground to the fineness of mixed material
It is 7-10 microns, component A is obtained after filtering.
(2) 1g dispersing agent WinSperse3050,42g conductive titanium dioxide is added in Xiang Shangshu component A, stirs 60min,
1500rpm obtains components I.
(3) acrylic resin (admittedly containing 46.5%) 40g is weighed, 0.6g dispersing agent WinSperse3050,8g titanium dioxide is added
Mechanical stirring 15min, revolving speed 800rpm, then grind 1h for the mixture again, and revolving speed 2000rpm is ground to fineness less than 25
Micron, obtains compositionⅱ after filtering.
(4) by components I, compositionⅱ and 1g anti-settling agent A630-SV, 0.77g levelling agent BYK-3550,1g defoaming agent BYK-
8821 are uniformly mixed, and obtain graphene static conductive priming paint 14.
Embodiment 15:
(1) 0.2g oleic acid is uniformly mixed with 50 milliliters of ethyl acetate, 50 milliliters of dehydrated alcohols, at 50 DEG C, 1000rpm is stirred
10min is mixed, 1g graphene and 0.5g carbon nanotube is added, 3000rpm is stirred to react 1h and washes after the completion of temperature 50 C stirring
It washs, filter, drying to get graphene complex is arrived.
(2) acrylic resin (admittedly containing 46.5%) 45.27g, dimethylbenzene 10g, mechanical stirring 10min, 1000rpm are weighed,
Then the compound of graphene and carbon nanotube obtained by 1.4g dispersing agent WinSperse330,0.6g step 1) is added, grinds 3h,
Revolving speed is 2000rpm, and the fineness for being ground to mixed material is 8-10 microns, and component A is obtained after filtering.
(3) 3.5g dispersing agent WinSperse3204,35g conductive titanium dioxide is added in Xiang Shangshu component A, stirs 30min,
1500rpm obtains components I.
(4) acrylic resin (admittedly containing 46.5%) 30g is weighed, 1.5g dispersing agent WinSperse3204,20g titanium white is added
Powder mechanical stirring 15min, revolving speed 800rpm, then grind 1h for the mixture again, and revolving speed 2000rpm is ground to fineness and is less than
25 microns, compositionⅱ is obtained after filtering.
(5) by components I, compositionⅱ and 2g anti-settling agent BYK-410,0.5g levelling agent Silok-8488,0.5g defoaming agent
Silok-4082 is uniformly mixed, and obtains graphene static conductive priming paint 15.
By the graphene priming paint electrostatic spraying prepared in embodiment 1-15 in plastic basis material and tinplate substrate surface.
After coating is dry, using the resistance of multimeter testing coating, using the L value of NR-10 type color difference meter testing coating, according to " GB/
T1733-1993 paint film water resistance measuring method " testing coating water resistance, according to " GB/T9286-1998 paint and varnish paint film
Cross cut test " testing coating adhesive force, according to the resistance to punching of " GB/T1732-1993 paint film impact resistance measuring method " testing coating
Hitting property.
Test result is as follows shown in table 1 for each embodiment graphene primer performance.
Table 1, graphene primer performance test result
From the analysis of upper the performance test results it is found that the resistance of graphene priming paint prepared by this technique is small, lightness is high, Er Qienai
Aqueous good, good mechanical property.
By the comparison of Fig. 1 and Fig. 2 it is found that according to a kind of patent " graphene of CN106009984A/acrylic acid static conductive coating
And preparation method thereof " preparation priming paint be ater, and the embodiment of the present invention 10 preparation gained priming paint of light color, the scope of application
It is wider.
Finally, it should be noted that the foregoing is only a preferred embodiment of the present invention, it is not intended to restrict the invention,
Although the present invention is described in detail referring to the foregoing embodiments, for those skilled in the art, still may be used
To modify the technical solutions described in the foregoing embodiments or equivalent replacement of some of the technical features.
All within the spirits and principles of the present invention, any modification, equivalent replacement, improvement and so on should be included in of the invention
Within protection scope.
Claims (11)
1. a kind of priming paint, each component including following mass parts: 35-55 parts of film forming matter, graphene or graphene complex
0.01-0.8 parts, 8-42 parts of complex conductive filler, 8-42 parts of titanium dioxide, dispersing agent I be 0.005-1.6 parts, dispersing agent II is
1.5-5 parts, 0.5-3 parts of auxiliary agent, 5-20 parts of solvent.
2. priming paint according to claim 1, it is characterised in that: the priming paint includes each component of following mass parts: film forming
0.1-0.5 parts of 40-50 parts of substance, graphene or graphene complex, 10-35 parts of complex conductive filler, titanium dioxide 10-35
Part, dispersing agent I are 0.05-1 parts, dispersing agent II is 2-4 parts, 1-2.5 parts of auxiliary agent, 5-15 parts of solvent；Alternatively,
The priming paint includes each component of following mass parts: 45-50 parts of film forming matter, graphene or graphene complex 0.05-
0.2 part, 25-35 parts of complex conductive filler, 12-25 parts of titanium dioxide, dispersing agent be I 0.02-0.2 parts, II 2.4-5 of dispersing agent
Part, 1.5-3 parts of auxiliary agent, 15-20 parts of solvent；
Specifically, the priming paint includes each component of following mass parts: 44.6 parts of film forming matter, graphene or graphene complex
0.2 part, 25 parts of complex conductive filler, 25 parts of titanium dioxide, dispersing agent I be 0.2 part, dispersing agent II be 3 parts, 2 parts of auxiliary agent, solvent
14.5 parts.
3. priming paint according to claim 1 or 2, it is characterised in that: the film forming matter is selected from acrylic resin, asphalt mixtures modified by epoxy resin
At least one of rouge, fluorocarbon resin and superchlorinated polyvinyl chloride resin；And/or
The graphene complex is the composite material by graphene and other carbon materials, other described carbon materials include carbon nanometer
Pipe and/or conductive black；And/or
The complex conductive filler is conductive titanium dioxide, conductive mica powder or conductive silica flour；The complex conductive filler
Preferably conductive titanium dioxide；And/or
The titanium dioxide is anatase thpe white powder；And/or the dispersing agent I is anionic, cationic, amphoteric or height
Molecule-type dispersing agent；And/or
The dispersing agent II is high-molecular type dispersing agent；And/or
The auxiliary agent is selected from least one of anti-settling agent, levelling agent and defoaming agent；And/or
The solvent is selected from toluene, dimethylbenzene, ethyl acetate, butyl acetate, N,N-dimethylformamide, N, N- dimethylacetamide
At least one of amine, dehydrated alcohol, isopropanol and dibutyl phthalate.
4. priming paint according to claim 3, it is characterised in that: in the film forming matter, the acrylic resin is attached most importance to
Molecular weight is the thermoplastic acrylic resin of 80000-90000；And/or
The epoxy resin is the epoxy resin of low epoxide number < 0.5；And/or
The fluorocarbon resin is the thermoplastic fluorocarbon resin that weight average molecular weight is 20000-50000；And/or
The superchlorinated polyvinyl chloride resin is middle low viscosity superchlorinated polyvinyl chloride resin；And/or
In the graphene complex, the mass fraction of graphene is 10%-90%；It is preferred that 30%-90%；And/or
Specifically, the method for preparing the graphene complex, comprising: pass through altogether graphene and carbon nanotube or conductive black
Mixed and/or modified technique is combined；
More specifically, the method for the graphene complex is prepared, comprising: graphite is added after mixing modifying agent and stirring solvent
Alkene and carbon nanotube or conductive black, are stirred to react and finish to obtain the final product；
Again specifically, in the modifying agent and stirring solvent mixing, speed of agitator 500-1000rpm；Mixing time is 10-
30min；Whipping temp is 50-100 DEG C；
It is described that being stirred to react in step of graphene and carbon nanotube or conductive black, speed of agitator 2000- is added
3000rpm；Reaction time is 0.5-2h；Reaction temperature is 50-100 DEG C；
The modifying agent is chosen in particular from least one of octadecylamine, dodecyl benzene sulfonic acid and oleic acid；And/or
The solvent is chosen in particular from least one of dimethylbenzene, ethyl acetate, N,N-dimethylformamide and dehydrated alcohol；
And/or
The dosage of the modifying agent is specially the 10%-20% of the gross mass of the graphene and carbon nanotube or carbon black；With/
Or,
In the dispersing agent I, anionic dispersing agent I in carboxylate, sulfuric ester, phosphate ester salt and sulfonate type at least
It is a kind of；And/or
Cationic dispersing agent I is selected from least one of alkyl quaternary ammonium salts, amino propylamine dioleate and quaternary ammonium salt；And/or
Amphoteric dispersing agent I is carboxylate；And/or
High-molecular type dispersing agent I is selected from least one of natural polymer dispersing agent and synthesis macromolecule dispersing agent；And/or
The dispersing agent I be chosen in particular from BYK163, BYK161, BYK110, BYK118, Disponer 9850,
SOLSPERSE37500、SOLSPERSE V350、SOLSPERSE20000、SOLSPERSE44000、S-601、Silok-7423、
Dispers 610S、S-4010B、DA-01、DA-168、DA-1040、Tech-6320、Tech-510、DA-703-50、
In WinSperse4900, WinSperse3030, WinSperse3050, WinSperse3300 and WinSperse3204 extremely
Few one kind；And/or
The dispersing agent II be chosen in particular from BYK163, BYK161, BYK110, DA-P10, DA-01, DA-168, DA-1040,
Tech-510、Disperbyk-180、WinSperse3030、WinSperse3050、WinSperse3300、
WinSperse3204, Dispex Ultra FA 4420, ZetaSperse 370, Sokalan CP 9, Ecodis P90 and
At least one of Tego Dispers 740W；And/or
In the auxiliary agent, anti-settling agent is N-Methyl pyrrolidone solution, modified hydrogenated castor oil, the titanate esters coupling of modified polyurea
Agent or polyamide wax；And/or
The relative molecular mass of the polyamide wax is specially 1500-3000；And/or
The anti-settling agent is chosen in particular from BYK-410, BYK-411, BYK-7411ES, FC-100, A630-SV, YB-301, EFKA
At least one of 3777N, DAPRO BEZ 75, NDZ-201 and GHDY920-20X；And/or
The levelling agent is organic silicon type levelling agent or esters of acrylic acid levelling agent；And/or
The levelling agent be chosen in particular from BYK-323, BYK-352, BYK-354, BYK-333, BYK-3550, Silok-8358,
At least one of Silok-8488 and EFKA 3777N；And/or
The defoaming agent is non-silicon class defoaming agent, polyethers defoaming agent or phosphoric acid ester defoaming agent；And/or
The defoaming agent is chosen in particular from BYK-017, BYK-018, BYK-051N, BYK-052N, BYK-1752, BYK-8821, B-
224、B-225、Foamaster MO 2190AC、Tego Foamex 3062、XIAMETER AFE-1430、Silok-4082、
At least one of Silok-4084 and Silok-4075；And/or
The mass ratio of the anti-settling agent, levelling agent and defoaming agent is 1.3-20:1:1-4；It is preferred that 2:1:1.
5. priming paint according to any one of claims 1-4, it is characterised in that: in the priming paint, the graphene or graphite
Piece-point-chip architecture conductive mesh that alkene compound, complex conductive filler and the graphene or graphene complex are formed
Network；Wherein, the complex conductive filler is inserted into the lamella of the graphene or graphene complex；And/or
The L value (lightness) of the priming paint is greater than 60；And/or
The sheet resistance of the priming paint is lower than 0.1M Ω.
6. a kind of preparation method of priming paint, using the component of proportional quantity in the priming paint any in claim 1-5, comprising:
It is first that part film forming matter is uniform with stirring solvent, it sequentially adds dispersing agent I and the graphene or graphene is compound
Object, grinding；
Part dispersing agent II and complex conductive filler are added, is stirred and evenly mixed, components I is obtained；
Remaining film forming matter, remaining dispersing agent II and titanium dioxide are stirred and evenly mixed, then mixture is ground, obtains component
Ⅱ；With
By the components I, the compositionⅱ and auxiliary agent be uniformly mixed to get.
7. according to the method described in claim 6, it is characterized by: the part film forming matter is the 30wt%- of film forming matter
75wt%；It is preferred that 50wt%；
The part dispersing agent II is the 20-75wt% of dispersing agent II；It is preferred that 50wt%.
8. method according to claim 6 or 7, it is characterised in that: the part film forming matter is uniformly walked with stirring solvent
In rapid, mixing time 10-20min, speed of agitator 400-1200rpm；Preferably, mixing time 15min, speed of agitator
For 1000rpm；
And/or in the grinding steps that dispersing agent I and the graphene or graphene complex is added, it is ground to mixture
The fineness of material is less than 10 microns；Preferably, milling time 2-5h, grinding revolving speed are 1500rpm-3500rpm；Preferably, it grinds
Time consuming is 3h, and grinding revolving speed is 2000rpm.
9. according to the method any in claim 6-8, it is characterised in that: addition part dispersing agent II and compound
After conductive filler the step of stirring and evenly mixing in, mixing time 20min-60min, speed of agitator 1000rpm-2000rpm；
Preferably, mixing time 30min, speed of agitator 1500rpm.
10. according to the method any in claim 6-9, it is characterised in that: it is described by remaining film forming matter, it is remaining
In the step of dispersing agent II and titanium dioxide stir and evenly mix, mixing time 10-20min, speed of agitator 200-1000rpm；It is preferred that
Ground, mixing time 15min；Speed of agitator is 800rpm；
And/or it is described remaining film forming matter, remaining dispersing agent II and titanium dioxide are stirred and evenly mixed after grinding steps in,
II fineness of obtained component is ground to less than 25 microns；Preferably, milling time 0.5-2h, grinding revolving speed are 1500rpm-
3500rpm；It is further preferred that milling time is 1h；Grinding revolving speed is 2000rpm.
11. any priming paint is preparing the application in static conductive priming paint in claim 1-5；And/or
Static conductive priming paint containing the priming paint any in claim 1-5.
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| CN115260851A (en) * | 2022-07-21 | 2022-11-01 | 江苏江南烯元石墨烯科技有限公司 | Preparation of conductive coating for cable bridge |
| CN115678362A (en) * | 2022-08-30 | 2023-02-03 | 江苏江南烯元石墨烯科技有限公司 | Transparent antistatic coating of single-walled carbon nanotube and preparation method thereof |
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