CN108281216A - A kind of watersoluble plumbago alkene heat-resistant fireproof electrocondution slurry and its preparation method and application - Google Patents
A kind of watersoluble plumbago alkene heat-resistant fireproof electrocondution slurry and its preparation method and application Download PDFInfo
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- CN108281216A CN108281216A CN201711420811.7A CN201711420811A CN108281216A CN 108281216 A CN108281216 A CN 108281216A CN 201711420811 A CN201711420811 A CN 201711420811A CN 108281216 A CN108281216 A CN 108281216A
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- watersoluble plumbago
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- 239000002002 slurry Substances 0.000 title claims abstract description 36
- -1 plumbago alkene Chemical class 0.000 title claims abstract description 35
- 239000010439 graphite Substances 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title abstract description 11
- 240000003936 Plumbago auriculata Species 0.000 title 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 94
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 93
- 238000000034 method Methods 0.000 claims abstract description 30
- 241000209456 Plumbago Species 0.000 claims abstract description 24
- 239000003063 flame retardant Substances 0.000 claims abstract description 24
- 229920005989 resin Polymers 0.000 claims abstract description 13
- 239000011347 resin Substances 0.000 claims abstract description 13
- 238000010438 heat treatment Methods 0.000 claims abstract description 9
- 238000012545 processing Methods 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 238000000576 coating method Methods 0.000 claims description 11
- 239000006185 dispersion Substances 0.000 claims description 11
- 239000003973 paint Substances 0.000 claims description 11
- 239000011248 coating agent Substances 0.000 claims description 10
- 230000000640 hydroxylating effect Effects 0.000 claims description 10
- 229910001868 water Inorganic materials 0.000 claims description 10
- 229910019142 PO4 Inorganic materials 0.000 claims description 9
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 9
- 239000010452 phosphate Substances 0.000 claims description 9
- DLYUQMMRRRQYAE-UHFFFAOYSA-N tetraphosphorus decaoxide Chemical compound O1P(O2)(=O)OP3(=O)OP1(=O)OP2(=O)O3 DLYUQMMRRRQYAE-UHFFFAOYSA-N 0.000 claims description 8
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 6
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 4
- 238000005229 chemical vapour deposition Methods 0.000 claims description 4
- 229910052710 silicon Inorganic materials 0.000 claims description 4
- 239000010703 silicon Substances 0.000 claims description 4
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 3
- 239000003822 epoxy resin Substances 0.000 claims description 3
- LNEPOXFFQSENCJ-UHFFFAOYSA-N haloperidol Chemical compound C1CC(O)(C=2C=CC(Cl)=CC=2)CCN1CCCC(=O)C1=CC=C(F)C=C1 LNEPOXFFQSENCJ-UHFFFAOYSA-N 0.000 claims description 3
- 229910052603 melanterite Inorganic materials 0.000 claims description 3
- 229920000647 polyepoxide Polymers 0.000 claims description 3
- 239000004814 polyurethane Substances 0.000 claims description 3
- 229920002635 polyurethane Polymers 0.000 claims description 3
- 239000004925 Acrylic resin Substances 0.000 claims description 2
- 229920000178 Acrylic resin Polymers 0.000 claims description 2
- 229910021577 Iron(II) chloride Inorganic materials 0.000 claims description 2
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 claims description 2
- 150000003839 salts Chemical class 0.000 claims description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-L Phosphate ion(2-) Chemical compound OP([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-L 0.000 claims 1
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims 1
- 229910052739 hydrogen Inorganic materials 0.000 claims 1
- 239000001257 hydrogen Substances 0.000 claims 1
- 238000012360 testing method Methods 0.000 description 20
- 239000000243 solution Substances 0.000 description 15
- 230000000694 effects Effects 0.000 description 11
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 9
- 239000002270 dispersing agent Substances 0.000 description 6
- 229910002804 graphite Inorganic materials 0.000 description 6
- 239000012752 auxiliary agent Substances 0.000 description 5
- 229910052799 carbon Inorganic materials 0.000 description 5
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 239000000853 adhesive Substances 0.000 description 4
- 230000001070 adhesive effect Effects 0.000 description 4
- 150000001721 carbon Chemical group 0.000 description 4
- 239000002131 composite material Substances 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 239000012528 membrane Substances 0.000 description 4
- 230000000979 retarding effect Effects 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 150000001336 alkenes Chemical class 0.000 description 3
- 238000005485 electric heating Methods 0.000 description 3
- 238000007306 functionalization reaction Methods 0.000 description 3
- 239000010410 layer Substances 0.000 description 3
- 239000003381 stabilizer Substances 0.000 description 3
- 238000010998 test method Methods 0.000 description 3
- 230000008901 benefit Effects 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 150000002118 epoxides Chemical class 0.000 description 2
- 230000009970 fire resistant effect Effects 0.000 description 2
- 125000002467 phosphate group Chemical group [H]OP(=O)(O[H])O[*] 0.000 description 2
- 229920003987 resole Polymers 0.000 description 2
- 239000004575 stone Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000002604 ultrasonography Methods 0.000 description 2
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 239000006004 Quartz sand Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 239000011231 conductive filler Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 239000011889 copper foil Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000007766 curtain coating Methods 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 210000004709 eyebrow Anatomy 0.000 description 1
- 210000000720 eyelash Anatomy 0.000 description 1
- 238000009408 flooring Methods 0.000 description 1
- 235000013312 flour Nutrition 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 1
- 229910000359 iron(II) sulfate Inorganic materials 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 238000007613 slurry method Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/24—Conductive material dispersed in non-conductive organic material the conductive material comprising carbon-silicon compounds, carbon or silicon
-
- 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
- C09D5/18—Fireproof paints including high temperature resistant paints
-
- 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B3/00—Ohmic-resistance heating
- H05B3/10—Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor
- H05B3/12—Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor characterised by the composition or nature of the conductive material
- H05B3/14—Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor characterised by the composition or nature of the conductive material the material being non-metallic
- H05B3/145—Carbon only, e.g. carbon black, graphite
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Dispersion Chemistry (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Manufacturing & Machinery (AREA)
- Paints Or Removers (AREA)
Abstract
The invention discloses a kind of methods preparing watersoluble plumbago alkene heat-resistant fireproof electrocondution slurry, and the method includes the steps 1) make surface include hydroxyl graphene processing；2) graphene uniform is dispersed in water-base resin.It also discloses the watersoluble plumbago alkene heat-resistant fireproof electrocondution slurry of the method preparation and watersoluble plumbago alkene heat-resistant fireproof electrocondution slurry is applied to prepare the purposes of the fire-retardant graphene Electric radiant Heating Film of aqueous high-temperature-resistant.
Description
Technical field
The invention belongs to field of graphene, specifically, the present invention relates to a kind of watersoluble plumbago alkene heat-resistant fireproof conductions
Slurry and preparation method thereof.
Background technology
Graphene is a kind of two-dimensional material being made of single layer of carbon atom, and wherein carbon atom is arranged in honeycomb lattice, graphite
The honeycomb structure of alkene is highly stable.When applying external force with graphene, carbon atomic layer meeting flexural deformation so that carbon atom need not weigh
It is new to arrange to adapt to external force, to which holding structure is stablized.It, will not be because of lattice defect when electronics in graphene moves in track
Or it introduces foreign atom and scatters.Since interatomic force is very strong, at normal temperatures, even if surrounding carbon atom occurs to squeeze
It hits, the interference that graphene internal electron is subject to is also very small, its electron mobility is more than 15000cm2/VS, electronics under room temperature
Movement velocity reached the 1/300 of the light velocity, it is higher than carbon nanotube or silicon crystal；And resistivity only has about 10-6 Ω cm,
It is lower than copper or silver, it is the material of current resistivity minimum.Since graphene has the above excellent performance, need to only add a small amount of
The electric conductivity of slurry can largely be improved.
But graphene is difficult to disperse in water-based system, current most of graphene conductive slurry is solvent type,
A degree of pollution can be caused to environment in use, and the health of people can be endangered.Existing watersoluble plumbago
Alkene electrocondution slurry is that a large amount of dispersant and stabilizer are added in system, so that graphene is stablized point using these auxiliary agents
It dissipates.But the presence of these auxiliary agents can seriously affect the electric conductivity of graphene, can not embody graphene as conductive filler
Advantage.Using auxiliary agent in water-based system dispersed graphite alkene, dispersion effect is poor, and graphene can reunite again when storing for a long time.Example
Such as, patent CN 104464883A disclose graphene conductive slurry, preparation method and the application of adsorption dispersant.For
Scattering problem is solved, surfactant and dispersant are introduced in system to help the evenly dispersed of graphene.But surface
Activating agent and dispersant itself are not involved in conduction, there is certain destruction to the electric conductivity of product prepared by slurry.Seriously
Affect the application and market development of graphene conductive slurry.
Patent CN 105898906A disclose it is a kind of using graphene aqueous slurry prepare Electric radiant Heating Film method describe one
Kind graphene aqueous slurry and the method for preparing Electric radiant Heating Film.The problem of this kind of scheme still has 1) use auxiliary agent dispersed graphite
Alkene；Dispersion effect is poor；2) Electric radiant Heating Film prepared does not have flame retardant effect, and there are security risks.It is aqueous that this method prepares graphene
Slurry is difficult to stablize storage for a long time, and prepared graphene Electric radiant Heating Film has great security risk, is easy to cause
Fire causes casualties.
Patent CN 105647549A disclose a kind of graphene fire-retardant film and its preparation method and application.This method is
Graphene oxide is mixed with fire retardant, prepares film forming.Then it is restored and graphene fire-retardant film is prepared.Party's legal system
Standby graphene fire-retardant film is added to a large amount of fire retardant, will seriously affect its electrical property and mechanical property, can not play stone
The advantage of black alkene.
As that studies graphene deepens continuously, graphene anti-static coatings, graphene Electric radiant Heating Film, the anti-electromagnetism of graphene
Curtain coating etc. constantly enters people’s lives.The safety of graphene Related product is increasingly paid close attention to by everybody.Especially stone
For black alkene electric heating products by large-scale application in warming, the safety of product is more important.Graphene electricity on the market at present
Hot product does not have flame retardant property, and hidden danger is huge.Therefore, graphene conductive slurry of the exploitation with flame retardant effect is compeled in eyebrow
Eyelash.
Invention content
By research, present inventors have proposed a kind of functionalization graphene with flame retardant effect, the graphene surfaces
Including hydroxyl.The graphene makes surface include hydroxyl by the processing of chemically or physically method, such as is grafted phosphate-based.
Therefore, on the one hand, the present invention provides a kind of method preparing watersoluble plumbago alkene heat-resistant fireproof electrocondution slurry,
The method includes the steps,
1) make surface include hydroxyl graphene processing, obtain hydroxylating graphene；
2) graphene uniform is dispersed in water-base resin.
In one embodiment, the graphene described in step 1) makes surface grafting by the processing of chemically or physically method
It is phosphate-based.In a specific embodiment, in step 1)：
1.a) by graphene dispersion to FeSO4·7H2O、FeCl2·4H2O、Fe(NO3)2·6H2O or H2O2Deng solution
In；
1.b) solution prepared is ultrasonically treated, makes graphene in the solution can be evenly dispersed；
1.c) scattered solution is poured into hydrothermal reaction kettle and is reacted.
In one embodiment, step 1.c) in hydrothermal reaction kettle in temperature be 180-220 DEG C.
In one embodiment, the graphene used in step 1) is each by redox, CVD method, mechanical stripping etc.
It is prepared by kind method
In one embodiment, the water-base resin described in step 2) is aqueous epoxy resins, resol resins, water
The one or more of property acrylic resin, aqueous polyurethane, waterborne organic silicon resin etc..
In one embodiment, in step 2)：
2.a) by the hydroxylating graphene dispersion being prepared in step 1) to phosphorus pentoxide water, phosphoric acid, phosphate, phosphorus
In sour monohydric salt or phosphate dihydrogen salt solution；
2.b) by step 2.a) in the solution that is prepared be ultrasonically treated, make graphene in the solution can be evenly dispersed；
2.c) by step 2.b) in scattered solution pour into hydrothermal reaction kettle and react.
In one embodiment, step 2.c) in hydrothermal reaction kettle in temperature be 90-110 DEG C.
At two aspects, the watersoluble plumbago alkene heat-resistant fireproof prepared the present invention provides the method for first aspect present invention is led
Plasma-based material, wherein graphene surface include hydroxyl, and the graphene uniform is dispersed in water-base resin.
In one embodiment, the graphene keeps surface grafting phosphate-based by the processing of chemically or physically method.
In one embodiment, the graphene is prepared by the various methods such as redox, CVD method, mechanical stripping.
In one embodiment, the water-base resin is aqueous epoxy resins, resol resins, water soluble acrylic acid tree
The one or more of fat, aqueous polyurethane, waterborne organic silicon resin etc..
In the third aspect, the present invention provides the watersoluble plumbago alkene heat-resistant fireproof electrocondution slurries of first aspect present invention
Applied to the purposes for preparing the fire-retardant graphene Electric radiant Heating Film of aqueous high-temperature-resistant.
In one embodiment, the purposes is applied to antistatic floor paint, electromagnetic screen coating.
The present invention uses water-based system, VOC free emission problem；Graphene used in the present invention is handled by hydroxylating,
Without auxiliary agent can in water system it is evenly dispersed；Graphene used in the present invention contain it is phosphate-based, without adding fire retardant
There can be excellent flame effect；The watersoluble plumbago alkene heat-resistant fireproof electrocondution slurry can work at 200 DEG C for a long time；It should
The fire-retardant rank of watersoluble plumbago alkene heat-resistant fireproof electrocondution slurry is V0 grades；The watersoluble plumbago alkene heat-resistant fireproof electrocondution slurry
Resistivity is 0.02-10 Ω cm.
Specific implementation mode
Present inventors have proposed a kind of watersoluble plumbago alkene heat-resistant fireproof electrocondution slurry, the watersoluble plumbago alkene heat-resistant fireproofs
The graphene that electrocondution slurry uses can be prepared by the various methods such as redox, CVD method, mechanical stripping, then passing through
It learns or physical method processing keeps graphene evenly dispersed in water-base resin and has high fire-retardance effect.
Existing watersoluble plumbago alkene electrocondution slurry all adds a large amount of dispersant in preparation process or stabilizer is used for
Ensure that graphene uniform and stable can disperse in water-based system.The mode of action of dispersant or stabilizer is to be coated on graphene
Sheet surfaces make it be not susceptible to reunite in water-based system.But this cladding form can greatly increase graphene sheet layer
Between contact resistance, so that the electric conductivity of electrocondution slurry is deteriorated.The graphene that the present invention uses makes after chemical method is handled
Graphene surface contains a certain amount of hydroxyl.The presence of hydroxyl enables graphene is uniform and stable to be dispersed in slurry system.
When graphene conductive product prepared by existing watersoluble plumbago alkene electrocondution slurry technology can only ensure long at 80 DEG C
Between use, which limits many application scenarios of electrocondution slurry.The graphene that the present invention uses after chemical method is handled,
Can significantly improve the heat resistance of watersoluble plumbago alkene conductive articles, highest can at 200 DEG C long-term stable work.
The flame retardant effect of the existing fire-retardant class product of graphene is realized by addition fire retardant.General fire retardant needs
Addition just has flame retardant effect when being more than 30wt%, and fire retardant can the serious electrical property for influencing product, mechanical performance at this time.
National coal changes under electric policy, and graphene electric heating product becomes the air port of graphene application.Addition fire retardant is made in the slurry
Standby product can seriously affect its electric conductivity again, can not be applied to electric heating.And the present invention is grafted resistance directly on graphene
Functional group is fired, enables graphene that there is excellent flame retardant effect again while ensureing its superior electrical conductivity.Prepared graphite
Alkene product can ensure excellent electrical property and flame retardant property simultaneously.
Embodiment
Prepare the processing step and work of the watersoluble plumbago alkene heat-resistant fireproof electrocondution slurry of one embodiment of the invention
Skill condition can be as follows：
1. the preparation of hydroxylating graphene
1.1) by graphene dispersion to FeSO4·7H2In the solution of O, wherein graphene：FeSO4·7H2O:Deionized water
Ratio be 1:(15-25):1；
1.2) the solution ultrasound 30min that will be prepared, makes graphene in the solution can be evenly dispersed；
1.3) scattered solution is poured into hydrothermal reaction kettle, reacts 4-6h at 200 DEG C, you can obtain hydroxyl graphite
Alkene.
2. the preparation of flame retarding function graphene
2.1) by the hydroxylating graphene dispersion to phosphorus pentoxide aqueous solution being prepared in step 1, wherein graphite
Alkene:Phosphorus pentoxide is (1-10):1；
2.2) the solution ultrasound 30min that will be prepared in step 2.1), makes graphene in the solution can be evenly dispersed；
2.3) scattered solution in step 2.2) is poured into hydrothermal reaction kettle, reacts 1-3h at 100 DEG C, you can obtain
Contain phosphate-based graphene.
3. the flame retarding function graphene is tested as follows：
3.1) hydroxylating graphene of the invention can stable dispersion 2 months in deionized water；Test method is as follows：It will
Hydroxylating graphene dispersion in deionized water, stands storage；The concentration of upper solution test graphene is taken after 2 months.With most
First configuration concentration is identical, then proves that hydroxylating graphene can stable dispersion in deionized water.
3.2) after functionalization graphene is mixed with aqueous high molecular material, the composite membrane of preparation can be stablized at 200 DEG C
Work；Test method is as follows：Prepared composite membrane is powered, its heating temperature is made to reach 200 DEG C.Persistently it is powered 30 days, it is multiple
The temperature for closing film does not change, it was demonstrated that composite membrane can the steady operation at 200 DEG C for a long time.
3.3) after functionalization graphene is mixed with aqueous high molecular material, the composite membrane of preparation after open fire calcination 30s according to
It will not so burn, the far super V0 ranks of flame retardant effect；Test method is as follows：Tested according to American Standard UL94-2013, to sample into
10 seconds twice combustion testings of row, flame can extinguish in 30 seconds, and no comburant is fallen down.
4. the flame retarding function graphene is used as antistatic floor paint, electromagnetic screen coating
4.1) the step of being used as antistatic floor paint is as follows：
A. cement flooring is cleaned out, it is desirable that dried flat；
B. it is laid with copper foil according to GBJ97 standards or copper wire, 10 ohm of ground resistance ＜ is spaced 2m*2m in length and breadth；
C. it uses watersoluble plumbago alkene heat-resistant fireproof slurry to match suitable quartz sand, is made into epoxide terrace paint middle level, blade coating reaches
To design thickness；
D.12h it uses watersoluble plumbago alkene heat-resistant fireproof slurry to configure appropriate silica flour afterwards, is configured to epoxide terrace paint surface layer,
Blade coating reaches design thickness, dry after 5 days to complete to can be obtained fire-resistant antistatic floor paint.
Prepared antistatic floor paint is tested as follows：
Adhesive force is tested, and carries out adhesive force test according to standard GB1720-79, test result is 0 grade.Impact resistance is surveyed
Examination carries out impact resistance test according to standard GB/T1732-1993, and test result is that can bear 1KG objects to fall in 1m eminences
Under impact.Wearability test is tested according to standard GB/T1768-1989, uses 750g counterweights turning in 500r/min
The lower loss of speed is 0.01g.Pencil hardness test is tested according to standard GB/T6739-1996, test result 2H.Surface
Resistance test is tested using sheet resistance instrument, test result 105Ω.Anti-flammability is tested, according to standard UL94-2013
It is tested, 10 seconds twice combustion testings is carried out to sample, flame can extinguish in 30 seconds, and no comburant is fallen down.
Prepared fire-resistant antistatic floor paint performance is much better than common floor paint, has extraordinary market prospects.
4.2) the step of being used as electromagnetic screen coating is as follows：
A., watersoluble plumbago alkene heat-resistant fireproof slurry is sprayed to the body surface for needing to be electromagnetically shielded using spray gun；
B. in one layer of protective topcoat of electromagnetic screen coating surface spraying
Prepared electromagnetic screen coating is tested as follows：
Conducting performance test, test result are that resistivity is 0.001 Ω cm.Capability of electromagnetic shielding is tested, according to standard
GJB6190-2008 is tested, and test result is that 10GHz wave band effectivenesses are 80dB.Adhesive force is tested, according to mark
Quasi- GB1720-79 carries out adhesive force test, and test result is 0 grade.Pencil hardness test, according to standard GB/T6739-1996 into
Row test, test result 2H.
Test result shows that the effectiveness of prepared electromagnetic screen coating is excellent, before having extraordinary market
Scape.
The flame retarding function graphene that can be seen that the present invention from the result is suitable as antistatic floor paint, electromagnetic screen
Cover coating.
Claims (10)
1. a kind of method preparing watersoluble plumbago alkene heat-resistant fireproof electrocondution slurry, the method includes the steps,
1) make surface include hydroxyl graphene processing, obtain hydroxylating graphene；
2) graphene uniform is dispersed in water-base resin.
2. according to the method described in claim 1, the graphene described in step 1) makes table by the processing of chemically or physically method
Face grafting is phosphate-based.
3. according to the method described in claim 1, in step 1)：
1.a) by graphene dispersion to FeSO4·7H2O、FeCl2·4H2O、Fe(NO3)2·6H2O、H2O2Deng solution in；
1.b) solution prepared is ultrasonically treated, makes graphene in the solution can be evenly dispersed；
1.c) scattered solution is poured into hydrothermal reaction kettle and is reacted.
4. according to the method described in claim 3, step 1.c) in hydrothermal reaction kettle in temperature be 180-220 DEG C.
5. according to the method described in claim 1, the graphene used in step 1) passes through redox, CVD method, mechanical stripping
It is prepared etc. various methods.
6. according to the method described in claim 1, the water-base resin described in step 2) is aqueous epoxy resins, aqueous phenolic aldehyde tree
The one or more of fat, water-based acrylic resin, aqueous polyurethane, waterborne organic silicon resin etc..
7. according to claim 1-5 any one of them methods, in step 2)：
2.a) by the hydroxylating graphene dispersion being prepared in step 1) to phosphorus pentoxide, phosphoric acid, phosphate, one hydrogen of phosphoric acid
In salt, biphosphate saline solution；
2.b) by step 2.a) in the solution that is prepared be ultrasonically treated, make graphene in the solution can be evenly dispersed；
2.c) by step 2.b) in scattered solution pour into hydrothermal reaction kettle and react.
8. watersoluble plumbago alkene heat-resistant fireproof electrocondution slurry prepared by claim 1-7 any one of them methods.
9. watersoluble plumbago alkene heat-resistant fireproof electrocondution slurry prepared by claim 1-6 any one of them methods is applied to prepare
The purposes of the fire-retardant graphene Electric radiant Heating Film of aqueous high-temperature-resistant.
10. purposes according to claim 9, the purposes is applied to antistatic floor paint, electromagnetic screen coating.
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