CN106883684A - Graphene three-dimensional composite water soluble electric heating ink and preparation method thereof - Google Patents
Graphene three-dimensional composite water soluble electric heating ink and preparation method thereof Download PDFInfo
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- CN106883684A CN106883684A CN201710211519.8A CN201710211519A CN106883684A CN 106883684 A CN106883684 A CN 106883684A CN 201710211519 A CN201710211519 A CN 201710211519A CN 106883684 A CN106883684 A CN 106883684A
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- 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
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- C09D11/52—Electrically conductive inks
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- 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
- C09D11/00—Inks
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- C09D11/03—Printing inks characterised by features other than the chemical nature of the binder
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Abstract
The present invention provides a kind of Graphene three-dimensional composite water soluble electric heating ink and preparation method thereof, including graphene dispersing solution, carbon nano tube dispersion liquid, carbon black dispersion liquid, the first water-base resin and the first dispersant so that Graphene, CNT, carbon black form three-dimensional stability structure；The method that carbon black and CNT form 3-D nano, structure layer is added by between Graphene and Graphene, the problem that the graphitization again that occurs after Electric radiant Heating Film long-time use, graphitization cause electric conversion efficiency to be decayed is solved；Carbon black is in granular form, and can regard zero dimensional nanometer materials as；CNT is in bar shape, belongs to monodimension nanometer material；Graphene is two-dimension nano materials in the form of sheets；This three classes material is combined together, and has been overlapped to form distinctive three-dimensional carbon nanometer heating body；Into skeleton network, a point contact is changed into from simple plane-plane contact, puts linear contact lay, line face contact, the mode that plane-plane contact is combined while increasing conductive path, improves back bone network resistance stability.
Description
Technical field
Preparation and applied technical field the invention belongs to nano composite material, are related to a kind of Graphene three-dimensional composite water soluble
Electric heating ink and preparation method thereof.
Background technology
Carbon series conductive ink with carbon black, graphite, carbon fiber and its mixture as main stuffing, because of with low cost, performance
Stably, the advantages of cost performance is high, is widely used in thin film switch, flexible circuit, medical electronics, communication apparatus in addition to Electric radiant Heating Film
With electromagnetic shielding etc. field.Inorganic nano metal system (such as copper system, silver system) and organic system (mostly conducting polymer) conductive oil
Ink has more excellent electric conductivity, therefore the novel ink filler such as nanometer conductive material and macromolecule conducting material gradually instead of
The leading research status of carbon conductive filler.
But with the discovery and application of carbon nanomaterial such as CNT and Graphene, prepared in this, as conductive agent new
Type carbon series conductive ink, with electrical conductivity higher, more excellent mechanical strength and lighter quality, with good Prospect of R ＆ D and
Market value.Traditional Electric radiant Heating Film uses conductive black and graphite as conductive agent, contact of the particle diameter between micron order, conductive agent
It is insufficient；In energization long-term use, unformed carbon black Long-term Vibration under the electric field action cause particle between contact knot
Structure is slack and undisciplined, and charge-conduction route can occur irreversible negative sense change, cause power attenuation；Using Graphene as conductive agent
Electrically conductive ink, if simple be susceptible to reunite by increasing Graphene quantity, and the easily cause graphitization that is layering, cause and lead
Electric pathway is reduced, and can also cause power attenuation, limits the useful life of traditional Electric radiant Heating Film.
The content of the invention
Regarding to the issue above, the present invention provides one kind three-dimensional composite water soluble electric heating ink of send out heat-staple Graphene.
To reach above-mentioned purpose, a kind of Graphene three-dimensional composite water soluble electric heating ink of the invention, it is characterised in that：Including stone
Black alkene, CNT, carbon black, the first water-base resin, the first dispersant and the second dispersant.
The present invention relates to one kind three-dimensional composite water soluble electric heating ink of send out heat-staple Graphene, received with carbon by the way that Graphene is first
Mitron is combined, then day acute hearing carbon black nano particle mode is set in gap so that Graphene, CNT and carbon black form three-dimensional
Rock-steady structure, and the graphitization again occurred after Electric radiant Heating Film long-time use is fundamentally solved the problems, such as, solve graphitization and lead
Send a telegraph the hang-up of thermal conversion efficiency decay.It is fastened to each other while condition each other, it is that free electron creates very big turnover
Space, reduces the graphitization effect again existed when Graphene works, and alleviates resistance decrement so that product heating property is permanent
Stabilization is kept, overcomes like product to use the problem of rear power attenuation for a long time.
Regarding to the issue above, the present invention provides a kind of preparation of three-dimensional composite water soluble electric heating ink of send out heat-staple Graphene
Method.
To reach above-mentioned purpose, a kind of preparation method of Graphene three-dimensional composite water soluble electric heating ink of the invention, its feature
It is to concretely comprise the following steps：
(1) Graphene ink point liquid is prepared：
(1) graphene powder of 0.1-10 weight portions is taken, is added with the speed of 5-10 weight portions/minute under stirring
Pure water 90-120 weight portions, are warming up to 25 DEG C~100 DEG C after addition, keep backspin stirring, thermostatic 10 hours；
(2) the first dispersant of 0.1-5 weight portions is added with the speed of 0.1-1 weight portions/minute, 25 is warming up to after addition
DEG C~100 DEG C, keep backspin stirring, thermostatic 46-50 hours；
(3) discharged after being cooled to normal temperature；
(2) multi-walled carbon nano-tubes ink point liquid is prepared：
(1) the multi-wall carbon nano-tube pipe powder of 4-10 weight portions is taken, with the speed of 5-10 weight portions/minute under stirring
Addition pure water 90-120 weight portions, are warming up to 25 DEG C~100 DEG C after addition, keep backspin stirring, thermostatic 10 hours；
(2) the second dispersant of 0.5-2 weight portions is added with the speed of 0.1-1 weight portions/minute, 25 is warming up to after addition
DEG C~100 DEG C, keep backspin stirring, thermostatic 46-50 hours；
(3) discharged after being cooled to normal temperature；
(3) carbon-loaded inks point liquid is prepared：
(1) hydrocarbon black powder of 0.1-10 weight portions is taken, the speed addition with 5-10 weight portions/minute under stirring is pure
Water purification 90-120 weight portions, are warming up to 25 DEG C~100 DEG C after addition, keep backspin stirring, thermostatic 46-50 hours；
(2) obtained carbon-loaded inks point liquid is filtered after being cooled to normal temperature, is filtered carbon black of the particle diameter more than 30nm
Grain.
(4) the multi-walled carbon nano-tubes ink point prepared in the Graphene ink that will be prepared in step (1) point liquid and (two)
Liquid is with 1：5 ratio is mixed, and obtains graphene-carbon nano tube mixed solution.
(5) carbon black oil prepared in the graphene-carbon nano tube mixed solution and step (3) that will be prepared in step (4)
Ink point liquid, obtains Graphene three-dimensional composite water soluble electric heating ink.
Further, in the step (4), including step：
(11) the multi-walled carbon nano-tubes oil obtained in the Graphene ink that will be obtained in step (1) point liquid and step (2)
Ink point liquid is according to 1：1 is mixed, and the first aqueous tree is added with the speed of 5-10 weight portions/minute in the mixed liquor that will be obtained
Fat, 70 DEG C~90 DEG C are at the uniform velocity warming up to 2-6 DEG C/min, keep 1500-2000rpm/min Stirrings, and constant temperature 0.8-1.5 is small
When；
(12) many wall carbon obtained in the graphene-carbon nano tube mixed liquor obtained in step (11) and step (2) are received
Mitron ink point liquid is according to 2：1 is mixed, and the first water is added with the speed of 5-10 weight portions/minute in the mixed liquor that will be obtained
Property resin, be at the uniform velocity warming up to 70 DEG C~90 DEG C with 2-6 DEG C/min, keep 1500-2000rpm/min Stirrings, constant temperature 0.8-
1.5 hours；
(13) many wall carbon obtained in the graphene-carbon nano tube mixed liquor obtained in step (12) and step (2) are received
Mitron ink point liquid is according to 3：1 is mixed, and the first water is added with the speed of 5-10 weight portions/minute in the mixed liquor that will be obtained
Property resin, be at the uniform velocity warming up to 70 DEG C~90 DEG C with 2-6 DEG C/min, keep 1500-2000rpm/min Stirrings, constant temperature 0.8-
1.5 hours.
Further, in the step (5), including step：
(21) carbon-loaded inks obtained in the graphene-carbon nano tube mixed liquor and step (3) that will be obtained in step (13)
Divide liquid according to 1:1 ratio is mixed, and 70 DEG C~90 DEG C are at the uniform velocity warming up to 2-6 DEG C/min, keeps 1500-2000rpm/min
Stirring, constant temperature 0.8-1.5 hours；
(22) the carbon-loaded inks point liquid obtained in the composite solution and step (3) that obtain step (21) is according to 2:1 ratio
Mixed, 70 DEG C~90 DEG C are at the uniform velocity warming up to 2-6 DEG C/min, kept 1500-2000rpm/min Stirrings, constant temperature
0.8-1.5 hours；
(23) the carbon-loaded inks point liquid obtained in the composite solution and step (3) that obtain step (22) is according to 2:1 ratio
Mixed, 70 DEG C~90 DEG C are at the uniform velocity warming up to 2-6 DEG C/min, kept 1500-2000rpm/min Stirrings, constant temperature
0.8-1.5 hours.
Further, the first dispersion liquid in the step (1) is the polysiloxane-based dispersant of machine Si modification, polycarboxylic acids
Sodium salt dispersant, the copolymer analog dispersant containing pigment affinity groups, from organic autohemagglutination carboxylic acid ammonium salt dispersant, quaternary ammonium salt
One or more in class dispersant and Sulfonates dispersant.
Further, the second dispersion liquid in the step (3) is polymethylacrylic acid, cetyl trimethyl bromination
Ammonium, neopelex, lauryl sodium sulfate, polyethylene glycol to isooctyl phenyl ether in one or more.
The present invention relates to a kind of preparation method of Graphene three-dimensional composite water soluble electric heating ink, first received with carbon by Graphene
Mitron is combined, then day acute hearing carbon black nano particle mode is set in gap so that Graphene, CNT and carbon black form three-dimensional
Rock-steady structure, this structure is fastened to each other while condition each other, and is that free electron creates very big turnover space, reduces
The graphitization effect again that Graphene exists when working, alleviates resistance decrement so that product heating property keeps stabilization for a long time, gram
Take like product and use the problem of rear power attenuation for a long time.
Reaction temperature that need not be very high using this reaction method, or even can be also obtained in the case of normal temperature, during reaction
Between decrease a lot, reduce energy consumption, save Production Time, save cost, improve efficiency, improve profit.
Brief description of the drawings
Fig. 1 be Graphene of the present invention three-dimensional composite water soluble electric heating ink it is microcosmic under picture；
Fig. 2 be Graphene of the present invention three-dimensional composite water soluble electric heating ink it is microcosmic under picture.
Specific embodiment
Implementation to specific embodiment of the invention below in conjunction with the accompanying drawings is further described.
Embodiment one
As shown in Figure 1-2, a kind of Graphene three-dimensional composite water soluble electric heating ink of the invention, it is characterised in that：Including graphite
Alkene dispersion liquid, carbon nano tube dispersion liquid, carbon black dispersion liquid, the first water-base resin, the first dispersant and the second dispersant.
First combined with CNT by Graphene, then day acute hearing carbon black nano particle mode is set in gap so that stone
Black alkene, CNT and carbon black form three-dimensional stability structure, and fundamentally solve what is occurred after Electric radiant Heating Film long-time use
Graphitization problem, solves the hang-up that graphitization causes electric conversion efficiency to be decayed again.These three materials form skeleton net
Network, a point contact is changed into from simple plane-plane contact, puts linear contact lay, and line face contact, the mode that plane-plane contact is combined, increase is led
While electric pathway, back bone network resistance stability is improve.It is fastened to each other while condition each other, it is that free electron is created
Very big turnover space, reduces the graphitization effect again existed when Graphene works, and alleviates resistance decrement so that product is sent out
Hot property keeps stabilization for a long time, overcomes like product to use the problem of rear power attenuation for a long time.
Embodiment two, a kind of preparation method of Graphene three-dimensional composite water soluble electric heating ink of the invention, it is characterised in that tool
Body step is：
(1) Graphene ink point liquid is prepared：
(1) graphene powder of 0.1-10 weight portions is taken, is added with the speed of 5-10 weight portions/minute under stirring
Pure water 90-120 weight portions, are warming up to 25 DEG C~100 DEG C after addition, keep backspin stirring, thermostatic 10 hours；
(2) the first dispersant of 0.1-5 weight portions is added with the speed of 0.1-1 weight portions/minute, 25 is warming up to after addition
DEG C~100 DEG C, keep backspin stirring, thermostatic 46-50 hours；
(3) discharged after being cooled to normal temperature；
(2) multi-walled carbon nano-tubes ink point liquid is prepared：
(1) the multi-wall carbon nano-tube pipe powder of 4-10 weight portions is taken, with the speed of 5-10 weight portions/minute under stirring
Addition pure water 90-120 weight portions, are warming up to 25 DEG C~100 DEG C after addition, keep backspin stirring, thermostatic 10 hours；
(2) the second dispersant of 0.5-2 weight portions is added with the speed of 0.1-1 weight portions/minute, 25 is warming up to after addition
DEG C~100 DEG C, keep backspin stirring, thermostatic 46-50 hours；
(3) discharged after being cooled to normal temperature；
(3) carbon-loaded inks point liquid is prepared：
(1) hydrocarbon black powder of 0.1-10 weight portions is taken, the speed addition with 5-10 weight portions/minute under stirring is pure
Water purification 90-120 weight portions, are warming up to 25 DEG C~100 DEG C after addition, keep backspin stirring, thermostatic 46-50 hours；
(2) obtained carbon-loaded inks point liquid is filtered after being cooled to normal temperature, is filtered carbon black of the particle diameter more than 30nm
Grain.
(4) the multi-walled carbon nano-tubes ink point prepared in the Graphene ink that will be prepared in step (1) point liquid and (two)
Liquid is with 1：5 ratio is mixed, and obtains graphene-carbon nano tube mixed solution.
(5) carbon black oil prepared in the graphene-carbon nano tube mixed solution and step (3) that will be prepared in step (4)
Ink point liquid, obtains Graphene three-dimensional composite water soluble electric heating ink.
First combined with CNT by Graphene, then day acute hearing carbon black nano particle mode is set in gap so that stone
Black alkene, CNT and carbon black form three-dimensional stability structure, and this structure is fastened to each other while condition each other, and is free electron
Very big turnover space is created, the graphitization effect again existed when Graphene works is reduced, resistance decrement is alleviated so that
Product heating property keeps stabilization for a long time, overcomes like product to use the problem of rear power attenuation for a long time.
Reaction temperature that need not be very high using this reaction method, or even can be also obtained in the case of normal temperature, during reaction
Between decrease a lot, reduce energy consumption, save Production Time, save cost, improve efficiency, improve profit.
Most preferred first dispersant dose is 2.5%, and most preferred first dispersant dose is 1.2%.
Preferable temperature is 50 DEG C -70 DEG C, and most preferred temperature is 60 DEG C.The most preferred reaction time is 48 hours.
Embodiment three, on the basis of above-described embodiment, in the step (4), including step：
(11) the multi-walled carbon nano-tubes oil obtained in the Graphene ink that will be obtained in step (1) point liquid and step (2)
Ink point liquid is according to 1：1 is mixed, and the first aqueous tree is added with the speed of 5-10 weight portions/minute in the mixed liquor that will be obtained
Fat, 70 DEG C~90 DEG C are at the uniform velocity warming up to 2-6 DEG C/min, keep 1500-2000rpm/min Stirrings, and constant temperature 0.8-1.5 is small
When；
(12) many wall carbon obtained in the graphene-carbon nano tube mixed liquor obtained in step (11) and step (2) are received
Mitron ink point liquid is according to 2：1 is mixed, and the first water is added with the speed of 5-10 weight portions/minute in the mixed liquor that will be obtained
Property resin, be at the uniform velocity warming up to 70 DEG C~90 DEG C with 2-6 DEG C/min, keep 1500-2000rpm/min Stirrings, constant temperature 0.8-
1.5 hours；
(13) many wall carbon obtained in the graphene-carbon nano tube mixed liquor obtained in step (12) and step (2) are received
Mitron ink point liquid is according to 3：1 is mixed, and the first water is added with the speed of 5-10 weight portions/minute in the mixed liquor that will be obtained
Property resin, be at the uniform velocity warming up to 70 DEG C~90 DEG C with 2-6 DEG C/min, keep 1500-2000rpm/min Stirrings, constant temperature 0.8-
1.5 hours.
Example IV, on the basis of above-described embodiment, in the step (5), including step：
(21) carbon-loaded inks obtained in the graphene-carbon nano tube mixed liquor and step (3) that will be obtained in step (13)
Divide liquid according to 1:1 ratio is mixed, and 70 DEG C~90 DEG C are at the uniform velocity warming up to 2-6 DEG C/min, keeps 1500-2000rpm/min
Stirring, constant temperature 0.8-1.5 hours；
(22) the carbon-loaded inks point liquid obtained in the composite solution and step (3) that obtain step (21) is according to 2:1 ratio
Mixed, 70 DEG C~90 DEG C are at the uniform velocity warming up to 2-6 DEG C/min, kept 1500-2000rpm/min Stirrings, constant temperature
0.8-1.5 hours；
(23) the carbon-loaded inks point liquid obtained in the composite solution and step (3) that obtain step (22) is according to 2:1 ratio
Mixed, 70 DEG C~90 DEG C are at the uniform velocity warming up to 2-6 DEG C/min, kept 1500-2000rpm/min Stirrings, constant temperature
0.8-1.5 hours.
Preferable temperature is 50 DEG C -70 DEG C, and most preferred temperature is 60 DEG C.The most preferred reaction time is 1 hour.
Embodiment five, on the basis of above-described embodiment, the first dispersion liquid in the step (1) is poly- for machine Si modification
Type siloxane dispersant, polycarboxylate sodium's class dispersant, the copolymer analog dispersant containing pigment affinity groups, from organic autohemagglutination carboxylic
One or more in acid ammonium salt class dispersant, quaternary ammonium salt dispersant and Sulfonates dispersant.
Embodiment six, on the basis of above-described embodiment, the second dispersion liquid in the step (3) is polymethyl
Acid, cetyl trimethylammonium bromide, neopelex, lauryl sodium sulfate, polyethylene glycol are to isooctyl phenyl
One or more in ether.
Embodiment eight, on the basis of above-described embodiment, the reaction temperature of step (132) is 25 DEG C~100 DEG C, during reaction
Between be 46-50 hour, stirring use lower Stirring.
Preferable temperature is 50 DEG C -70 DEG C, and most preferred temperature is 60 DEG C.The most preferred reaction time is 48 hours.
Embodiment nine, on the basis of above-described embodiment, in the step (2), including step：
(211) CNT obtained in the graphene dispersing solution and step (122) that will be obtained in step (112) disperses heat
According to 1：1 is mixed, and adds the first water-base resin in the mixed liquor that will be obtained, and reaction temperature is 70 DEG C~90 DEG C, is stirred and is
1500-2000rpm/min high speed Stirrings, the reaction time is 0.8-1.5 hours；
(212) carbon obtained in the graphene-carbon nano tube mixed solution and step (122) that will be obtained in step (211)
Nanotube disperses according to 2：1 is mixed, and the first water-base resin is added in the mixed liquor that will be obtained, and reaction temperature is 70 DEG C~90
DEG C, it is 1500-2000rpm/min high speed Stirrings to stir, and the reaction time is 0.8-1.5 hours；
(213) carbon obtained in the graphene-carbon nano tube mixed solution and step (122) that will be obtained in step (212)
Nanotube disperses according to 3：1 is mixed, and the first water-base resin is added in the mixed liquor that will be obtained, and reaction temperature is 70 DEG C~90
DEG C, it is 1500-2000rpm/min high speed Stirrings to stir, and the reaction time is 0.8-1.5 hours.
Graphene dispersing solution and carbon nano tube dispersion liquid mixing add carbon nano tube dispersion liquid by several times, enable to mixing more
Plus fully, CNT can be inserted at a high speed between graphene sheet layer, make simple plane-plane contact be changed into sufficiently being converted into line
Face contacts.
Embodiment ten, on the basis of above-described embodiment, in the step (2), including step：
(311) charcoal obtained in the graphene-carbon nano tube mixed solution and step (133) that will be obtained in step (213)
Black dispersion liquid is according to 1:1 ratio is mixed, and reaction temperature is 70 DEG C~90 DEG C, is stirred as 500-800rpm/min middling speeds rotate
Stirring, the time is 0.5-1.0 hours；
(312) carbon black dispersion liquid obtained in the composite solution and step (133) that obtain step (311) is according to 2:1 ratio
Example is mixed, and reaction temperature is 70 DEG C~90 DEG C, and it is 500-800rpm/min middling speed Stirrings to stir, and the time is 0.5-
1.0 hours；
(313) carbon black dispersion liquid obtained in the composite solution and step (133) that obtain step (312) is according to 2:1 ratio
Example is mixed, and reaction temperature is 70 DEG C~90 DEG C, and it is 500-800rpm/min middling speed Stirrings to stir, and the time is 0.8-
1.5 hours.
In the addition graphene-carbon nano tube mixed solution of carbon black dispersion liquid gradation, enable to be more fully mixed, carbon
Nanotube can be inserted at a high speed between graphene sheet layer, make simple plane-plane contact be changed into sufficiently being converted into a point contact, point
Linear contact lay, line face contact, the mode that face contact is combined while increasing conductive path, improves back bone network resistance stabilization
Property.
More than, only presently preferred embodiments of the present invention, but protection scope of the present invention is not limited thereto, any to be familiar with sheet
Those skilled in the art the invention discloses technical scope in, the change or replacement that can be readily occurred in should all be covered
Within protection scope of the present invention.Therefore, the protection domain that protection scope of the present invention should be defined by claim is defined.
Claims (6)
1. a kind of Graphene three-dimensional composite water soluble electric heating ink, it is characterised in that：Including Graphene, CNT, carbon black, first
Water-base resin, the first dispersant and the second dispersant.
2. the preparation method of a kind of Graphene three-dimensional composite water soluble electric heating ink, it is characterised in that concretely comprise the following steps：
(1) Graphene ink point liquid is prepared：
(1) graphene powder of 0.1-10 weight portions is taken, the speed addition with 5-10 weight portions/minute under stirring is pure
Water 90-120 weight portions, are warming up to 25 DEG C~100 DEG C after addition, keep backspin stirring, thermostatic 10 hours；
(2) the first dispersant of 0.1-5 weight portions is added with the speed of 0.1-1 weight portions/minute, be warming up to after addition 25 DEG C~
100 DEG C, keep backspin stirring, thermostatic 46-50 hours；
(3) discharged after being cooled to normal temperature；
(2) multi-walled carbon nano-tubes ink point liquid is prepared：
(1) the multi-wall carbon nano-tube pipe powder of 4-10 weight portions is taken, is added with the speed of 5-10 weight portions/minute under stirring
Pure water 90-120 weight portions, are warming up to 25 DEG C~100 DEG C after addition, keep backspin stirring, thermostatic 10 hours；
(2) the second dispersant of 0.5-2 weight portions is added with the speed of 0.1-1 weight portions/minute, be warming up to after addition 25 DEG C~
100 DEG C, keep backspin stirring, thermostatic 46-50 hours；
(3) discharged after being cooled to normal temperature；
(3) carbon-loaded inks point liquid is prepared：
(1) hydrocarbon black powder of 0.1-10 weight portions is taken, pure water is added with the speed of 5-10 weight portions/minute under stirring
90-120 weight portions, are warming up to 25 DEG C~100 DEG C after addition, keep backspin stirring, thermostatic 46-50 hours；
(2) obtained carbon-loaded inks point liquid is filtered after being cooled to normal temperature, is filtered carbon black pellet of the particle diameter more than 30nm.
(4) the multi-walled carbon nano-tubes ink point liquid prepared in the Graphene ink that will be prepared in step (1) point liquid and (two) with
1：5 ratio is mixed, and obtains graphene-carbon nano tube mixed solution.
(5) carbon-loaded inks point prepared in the graphene-carbon nano tube mixed solution and step (3) that will be prepared in step (4)
Liquid, obtains Graphene three-dimensional composite water soluble electric heating ink.
3. the preparation method of Graphene according to claim 2 three-dimensional composite water soluble electric heating ink, it is characterised in that described
In step (4), including step：
(11) the multi-walled carbon nano-tubes ink point obtained in the Graphene ink that will be obtained in step (1) point liquid and step (2)
Liquid is according to 1：1 is mixed, and the first water-base resin is added with the speed of 5-10 weight portions/minute in the mixed liquor that will be obtained, with
2-6 DEG C/min is at the uniform velocity warming up to 70 DEG C~90 DEG C, keeps 1500-2000rpm/min Stirrings, constant temperature 0.8-1.5 hours；
(12) multi-walled carbon nano-tubes obtained in the graphene-carbon nano tube mixed liquor and step (2) that will be obtained in step (11)
Ink point liquid is according to 2：1 is mixed, and the first aqueous tree is added with the speed of 5-10 weight portions/minute in the mixed liquor that will be obtained
Fat, 70 DEG C~90 DEG C are at the uniform velocity warming up to 2-6 DEG C/min, keep 1500-2000rpm/min Stirrings, and constant temperature 0.8-1.5 is small
When；
(13) multi-walled carbon nano-tubes obtained in the graphene-carbon nano tube mixed liquor and step (2) that will be obtained in step (12)
Ink point liquid is according to 3：1 is mixed, and the first aqueous tree is added with the speed of 5-10 weight portions/minute in the mixed liquor that will be obtained
Fat, 70 DEG C~90 DEG C are at the uniform velocity warming up to 2-6 DEG C/min, keep 1500-2000rpm/min Stirrings, and constant temperature 0.8-1.5 is small
When.
4. the preparation method of Graphene according to claim 2 three-dimensional composite water soluble electric heating ink, it is characterised in that described
In step (5), including step：
(21) the carbon-loaded inks point liquid obtained in the graphene-carbon nano tube mixed liquor and step (3) that will be obtained in step (13)
According to 1:1 ratio is mixed, and 70 DEG C~90 DEG C are at the uniform velocity warming up to 2-6 DEG C/min, keeps 1500-2000rpm/min rotations
Stirring, constant temperature 0.8-1.5 hours；
(22) the carbon-loaded inks point liquid obtained in the composite solution and step (3) that obtain step (21) is according to 2:1 ratio is carried out
Mixing, 70 DEG C~90 DEG C are at the uniform velocity warming up to 2-6 DEG C/min, keep 1500-2000rpm/min Stirrings, constant temperature 0.8-1.5
Hour；
(23) the carbon-loaded inks point liquid obtained in the composite solution and step (3) that obtain step (22) is according to 2:1 ratio is carried out
Mixing, 70 DEG C~90 DEG C are at the uniform velocity warming up to 2-6 DEG C/min, keep 1500-2000rpm/min Stirrings, constant temperature 0.8-1.5
Hour.
5. the first dispersion liquid in step (1) described in is the polysiloxane-based dispersant of machine Si modification, polycarboxylate sodium's class is disperseed
Agent, the copolymer analog dispersant containing pigment affinity groups, from organic autohemagglutination carboxylic acid ammonium salt dispersant, quaternary ammonium salt dispersant and
One or more in Sulfonates dispersant.
6. the second dispersion liquid in step (3) described in is polymethylacrylic acid, cetyl trimethylammonium bromide, dodecyl
Benzene sulfonic acid sodium salt, lauryl sodium sulfate, polyethylene glycol to isooctyl phenyl ether in one or more.
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