CN109587842A - A kind of graphene-based self limiting temperature electric heating slurry and preparation method thereof and the application in electric heating floor system - Google Patents
A kind of graphene-based self limiting temperature electric heating slurry and preparation method thereof and the application in electric heating floor system Download PDFInfo
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- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 126
- 238000005485 electric heating Methods 0.000 title claims abstract description 93
- 239000002002 slurry Substances 0.000 title claims abstract description 57
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 238000007613 slurry method Methods 0.000 title abstract description 5
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- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 2
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- JDSQBDGCMUXRBM-UHFFFAOYSA-N 2-[2-(2-butoxypropoxy)propoxy]propan-1-ol Chemical compound CCCCOC(C)COC(C)COC(C)CO JDSQBDGCMUXRBM-UHFFFAOYSA-N 0.000 description 1
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- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- 229910021502 aluminium hydroxide Inorganic materials 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- RUFJMLKBWUXJMX-UHFFFAOYSA-N barium;carbonic acid Chemical compound [Ba].OC(O)=O RUFJMLKBWUXJMX-UHFFFAOYSA-N 0.000 description 1
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Classifications
-
- 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
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F24—HEATING; RANGES; VENTILATING
- F24D—DOMESTIC- OR SPACE-HEATING SYSTEMS, e.g. CENTRAL HEATING SYSTEMS; DOMESTIC HOT-WATER SUPPLY SYSTEMS; ELEMENTS OR COMPONENTS THEREFOR
- F24D13/00—Electric heating systems
- F24D13/02—Electric heating systems solely using resistance heating, e.g. underfloor heating
- F24D13/022—Electric heating systems solely using resistance heating, e.g. underfloor heating resistances incorporated in construction elements
- F24D13/024—Electric heating systems solely using resistance heating, e.g. underfloor heating resistances incorporated in construction elements in walls, floors, ceilings
-
- 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
- H05B3/20—Heating elements having extended surface area substantially in a two-dimensional plane, e.g. plate-heater
-
- 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
- H05B2203/00—Aspects relating to Ohmic resistive heating covered by group H05B3/00
- H05B2203/017—Manufacturing methods or apparatus for heaters
Landscapes
- Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Combustion & Propulsion (AREA)
- Mechanical Engineering (AREA)
- General Engineering & Computer Science (AREA)
- Surface Heating Bodies (AREA)
- Floor Finish (AREA)
Abstract
Application the invention discloses a kind of graphene-based self limiting temperature electric heating slurry and preparation method thereof and in electric heating floor system.The electric heating slurry is to prepare homogeneous graphene Multi-function electric heating slurry with after being mixed comprising graphene dispersing solution, resin, electric heating filler, PTC self limiting temperature filler, function of removing formaldehyde filler, each analog assistant；After wooden substrate surface treatment, pure graphene slurry is coated to promote each surface heating conduction of substrate；By Multi-function electric heating slurry, substrate carries out compound, laying conducting wire, protective layer, insulating layer and temperature control system etc. after drying with treated.The present invention has heating layer self limiting temperature, function of removing formaldehyde, and substrate high thermal conductivity, manufacturing process is simple, health environment-friendly, the advantages that being produced on a large scale.
Description
Technical field
The present invention relates to a kind of graphene-based self limiting temperature electric heating slurry and preparation method thereof and in electric heating floor system
Using belonging to thermo electric material and application field.
Background technique
Atmosphere pollution caused by problem of environmental pollutions such as " hazes " cause the great attention of the whole society, tradition coal-fired, also
One of the Major Risk Factors of China Public health are influenced through becoming, and cause hundred billion healthy economy loss and disease to China every year
Disease burden.China is second-biggest-in-the-world electricity consumption state, installed capacity the first in the world.Electric heating is promoted the use of, coal-fired supply is substituted
It is warm, it is possible to reduce pollutant emission.Electric heating floor is the composite floor board that can be generated heat after a kind of energization, by conductive special electric heating
Slurry, metal current-carrying item are processed, are compounded on insulation wood based substrate material and are made.Using electro-thermal coatings as heater when work,
Heat is sent into space in the form of radiation, obtains human body and object first warm, resultant effect is better than traditional convection current
Heating system.Electric heating system is by power supply, temperature controller, wearing layer, decorative layer, substrate layer, graphene-based conductive heating layer, protective layer
And the forming composite structures such as heat preservation reflecting layer.Power supply is connected to conductive heating layer through conducting wire, converts electrical energy into thermal energy.Due to conduction
Heating layer is pure resistor element circuit, therefore its high conversion efficiency, and except fraction loss (2%), most (98%) is converted to thermal energy.
Compared with traditional coal heating mode, has many advantages, such as heat supply choosing that is healthy, environmentally friendly, energy saving, high-efficient, and can provide personalized
It selects, is expected to solve pollution sources from the root, it is imperative.
Graphene is the emerging carbon material being made of honeycomb single layer of carbon atom layer, has excellent electric property (electronics
Mobility > 2 × 105 cm2/ V s), heating conduction (5000 W/mK) outstanding, specific surface area (2630 m of superelevation2/ g),
Also have both simultaneously light, flexibility is good, can large area the advantages that using, is not oxidizable, have more more prominent than other thermo electric materials
Far-infrared radiated property out, manufactured heating component has the characteristics that sendible temperature is high, thermal comfort is good, therefore has into
The characteristics of for excellent thermo electric material and potentiality.
Although 106304435 A of Chinese patent CN 108177225 A, CN 107559938 A, CN has used graphene
As electric heating slurry core component, but its safety it is anti-cross thermal design all rely on anti-overheat temperature control device, i.e., dependent on temperature pass
Sensor (thermocouple) measures temperature and preset temperature controls program, and this depends on the placement location of temperature sensor.Temperature
Sensor placement location it is unreasonable or far from thermocouple placement location regional temperature it is excessively high when, easily initiation hot-spot without
It is controlled by temperature program, causes fire.Reach itself limit Wen Gong by the regulation to graphene electric heating paste composition and function
The research and development of energy, have not been reported yet.
Existing graphene or graphite-like electric heating slurry and its electric heating application, such as 205279216 U of Chinese patent CN,
107882294 A of CN107178819 A, CN etc., although graphene is used to be coated on basis material as electric heating application,
It coats range and is only limitted to basis material side, just with graphene resistance heating function, fails that graphene is made full use of to go out
The heat of substrate side is transferred to the other side by the way that circumferential surface is graphene coated by the heat transfer character of color, and graphene is excellent
Thermal conducting function fails to be fully used, and leads to have considerable part heat to fail to be transferred to floor surface and be wasted.
Summary of the invention
The present invention is intended to provide a kind of graphene-based self limiting temperature electric heating slurry and preparation method thereof and in electric heating floor system
In application pass through graphene and each functional stuffing, self limiting temperature filler to have the graphene of excellent physicochemical property as raw material
Liquid phase it is compound, make it have electric fever, infrared emission, it is fire-retardant, except formaldehyde, self limiting temperature, resistivity, operating voltage and the function that generates heat
The functions such as rate is adjustable.
The present invention also provides the preparation methods of the electric heating slurry and its application in electric heating floor system.By to base
Material all surface is coated with pure graphene, using its excellent thermal conducting function, keeps the heat of graphene conductive heating layer high
Effect is transferred to substrate another side, improves heat utilization ratio.
The present invention provides a kind of graphene-based self limiting temperature electric heating slurry, the raw material including following weight proportion:
Graphene: 1-20 parts,
Dispersion liquid solvent: 10-500 parts,
Resin: 10-50 parts,
Electric heating filler: 0.5-10 parts,
Self limiting temperature PTC(has the self limiting temperature material of positive temperature coefficient) filler: 1-20 parts,
Functional stuffing: 0-5 parts,
Dispersing agent: 0-0.5 parts,
Defoaming levelling agent: 0-0.5 parts；
Above-mentioned raw materials prepare graphene-based self limiting temperature electric heating slurry after being mixed.
In above-mentioned graphene-based self limiting temperature electric heating slurry, the graphene is powder or liquid slurry；Graphene microchip contains
There are one or more of hydroxyl, carboxyl, amino, nitro functions；5 nm of graphene thickness <, lateral dimension 0.5~100
μm, crystal structure is complete；
Dispersion liquid solvent used includes one of water, alcohol solvent, ketone solvent, alcohol ethers solvent；
The resin includes water-based acrylic resin lotion, aqueous polyurethane resin emulsion, polymethyl methacrylate, melamine
One of amine-formaldehyde resins；
The electric heating filler includes the mixture of one or more of carbon nanotube, conductive black, electrically conductive graphite；
The self limiting temperature PTC filler includes one of barium carbonate base ceramic PTC, boronation titanium-based PTC, polymer resin base PTC；
It is 0.5-10 μm that self limiting temperature PTC filler, which is through one of ball milling, sand milling or spray drying or the obtained partial size of any combination,
Filler particles；
The functional stuffing includes the mixture except one or more of formaldehyde filler, fire-retardant filler, infrared reinforcing filler；
The formaldehyde filler that removes includes cold catalyst, MHCC material, without one of photocatalyst, MHCC material (Multifunctional
High Performance Confined Catalysis) it is to select high-specific surface area active material for substrate, it is soaked through active liquid
Efficient catalyst made from microwave treatment after stain；Fire-retardant filler includes magnesium hydroxide, one of aluminium hydroxide；Infrared reinforcing filler
Include one of zirconium oxide, zinc oxide；
The dispersing agent includes neopelex, polyalcohol, neopelex, burnt grace acid sodium, polyoxy second
One of alkene octyl phenyl ether, carboxymethyl cellulose；
The defoaming levelling agent includes polyether modified silicon oil, fluoro-acrylate copolymer, polyether-modified polydisiloxane, hard
One of fatty acid amide, aluminum stearate.
The present invention provides the preparation methods of above-mentioned graphene-based self limiting temperature electric heating slurry, comprising the following steps:
(a) graphene powder or dispersions in liquids for choosing different sizes, thickness, carry out pre-dispersed；
(b) resin, electric heating filler, self limiting temperature PTC filler, functional stuffing, dispersing agent, defoaming levelling agent are added and is stirred in proportion
It mixes, after being dispersed with stirring 1-3h, carries out grinding 0.5h ~ 6h, after being ground to granularity less than 50 microns, homogenous disperse liquid is obtained, to this
Homogenous disperse liquid carries out sieving processing, removes remaining reunion graphene and undissolved auxiliary agent on sieve, be made it is graphene-based from
Limit warm electric heating slurry.
Above-mentioned preparation method, specifically, pre-dispersed described in step a) use ultrasonic disperse or compound point of mechanical stirring
The mode of dissipating；Lapping mode used in step b) includes one of mechanical ball mill, sand mill grinding, three-roll grinder grinding or any
Kind combination；It is described sieving processing sieve mesh number be 300-400 mesh (sieve of this size can just remove reunion graphene with
Undissolved auxiliary agent).
The present invention provides application of the above-mentioned graphene-based self limiting temperature electric heating slurry in electric heating floor system.
In above-mentioned application, core electric heating layer is prepared using graphene-based self limiting temperature electric heating slurry, with other each layers (including
Wearing layer, decorative layer, substrate layer, protective layer, heat preservation reflecting layer) compound prepare electric heating floor.The floor system is from top to bottom
It successively include wearing layer, decorative layer, substrate layer, graphene-based conductive heating layer, protective layer, heat preservation reflecting layer.
Specifically, the wearing layer is by addition aluminum oxide resin or addition aluminum oxide overlay paper dipping three
Cymel composition；
The decorative layer is one of melamine facing paper, PVC, decoration veneer；
The substrate layer is one of high-density plate, medium-density plate, particieboard, solid wood board；
The heat preservation reflecting layer is flame retardant type molded polystyrene foams plate (EPS), extruded sheet (XPS), in polyethylene board
It is a kind of；Insulating layer is equipped with aluminium foil reflecting layer close to protective layer side.
In above-mentioned application, the preparation process of electric heating floor is as follows:
(1) wood substrate is surface-treated；
(2) each surface of wood substrate is covered into pure graphite ene coatings；
(3) drying and processing；
(4) graphene-based electric heating slurry is carried out being compounded to form graphene conductive fever with the wood substrate for being coated with pure graphene
Layer；
(5) it is dried；
(6) conductive metal lines are laid with and install temperature control sensor；
(7) armor coated.
Further, the preparation process of electric heating floor is specific as follows: (1) being surface-treated to wood substrate；Described
Surface treatment, which refers to, improves surface of wooden substrate active force using mechanical surface polishing, plasma technique or sided corona treatment method,
Strengthening slurry binding force；
(2) six surfaces of cuboid wood substrate are covered into pure graphite ene coatings；
The graphite ene coatings refer to pure graphene aqueous liquid dispersion, and the concentration of pure graphene aqueous liquid dispersion is 5 mg/mL
– 50 mg/mL；The surface covering, which refers to, coats graphene coating uniform using the technique in spraying, being immersed in；
(3) drying and processing, no less than 60 minutes are carried out under 60-120 °C；
(4) graphene-based electric heating slurry is subjected to combination process with the wood substrate for being coated with pure graphene, forms graphene and leads
Electric heating layer；The shape of conductive heating layer is latticed or dentation；Conductive heating layer with a thickness of 5-50 μm；Resistivity value is 0
.2-200 Ω·cm；
Compound includes one of printing, roll marks, spraying process；
(5) it is dried: one of dry using closed oven drying, the drying of infrared light irradiation, thermal convection drying, UV；
(6) conductive metal lines are laid with and install temperature control sensor；Temperature control sensor includes temperature sensor and overheat protector；
Conductive metal includes the combination of one or more of copper-foil conducting electricity, conductive copper paste, conducting aluminum paste and conductive silver paste；Conductive gold
The thickness of the thickness and electric heating slurry that belong to track laying is close, and the two thickness difference is at ± 10 μm；
(7) armor coated: protective layer is in polyurethane, ABS resin, polyamide, polysulfones, polyimides or polyetherimide
One kind, coating processes include printing, blade coating, spraying one of, coating thickness be 0.03-0.3 mm.
In above-mentioned application, the electric heating operating voltage of electric heating floor is 10-220 V；Steady state operating temperature is 30-95 °
C。
Beneficial effects of the present invention:
(1) use removing high-quality graphene in situ for electric heating material, compared with other carbon materials, graphene has lower
Thermo electric material weight can be effectively reduced in specific gravity, can be used with large area；Graphene has excellent mechanical property and good
Electric conductivity, machinability are high；The graphene coefficient of heat conduction with higher, can quickly distribute heat, and temperature is uniform and stable,
Long service life.
(2) by increasing PTC self limiting temperature filler in electric heating slurry ingredients, by its distinctive resistance coefficient with temperature liter
High and increase characteristic, the electric heating slurry have under no temperature control sensor and control procedure condition, and automatic temp limit controls power
Characteristic, conductive heating layer safety can be greatly improved, avoid because temperature sensor be arranged unreasonable or other reasons cause
Hot-spot and generate the hidden danger of fire.
(3) by increase in slurry ingredients including except the functional filler including formaldehyde filler, can provide except formaldehyde,
The functional applications such as fire-retardant, infrared enhancing transmitting, safety and environmental protection.
(4) resistivity is adjustable after electric heating slurry is dry, is adapted to different operating voltage, especially can be in human-body safety
Operating at voltages, while functional filler can be added, increase and inhibit bacterium, increase the function of infra-red radiation, release 6-14 is micro-
The far infrared of rice, human body, which easily absorbs, to be approached, and physiotheraping effect is obvious.
(5) graphene covering is carried out to all surface of wood substrate, makes full use of graphene superior thermal conductivity matter, it will
Substrate and the heat of conductive heating layer side are transferred to the other side by the graphene that circumferential surface coats, and utilize to greatest extent
Electric heating avoids partial heat from failing to be transferred to floor surface and be wasted.Realize that electric heating floor is energy-saving, heat dissipation is uniform, knot
The functions such as structure stabilization.
Detailed description of the invention
Fig. 1 is that projection Electronic Speculum (TEM) photo of raw graphite alkene microplate and scanning electron microscope (SEM) are shone in embodiment 1 and 4
Piece.Wherein a, c are the TEM photo of raw graphite alkene microplate, and b, d are scanning electron microscope sem photo.The difference of a/c, b/d are
Graphene raw material used is prepared by different methods: a, b are the graphenes prepared in embodiment 1；C, d are prepared in embodiment 4
Graphene.Two kinds of graphenes can be used as raw material in the technical scheme.
Fig. 2 (a) is that each interlayer relative position in high thermal conductivity self limiting temperature floor made of graphene-based self limiting temperature electric heating slurry shows
It is intended to, (b) is coated with graphene schematic diagram for each surface of wood substrate.
Specific embodiment
The present invention is further illustrated below by embodiment, but is not limited to following embodiment.
Embodiment 1:
Grapheme material is prepared using electrochemistry swelling graphite electrode method, graphene is about with a thickness of 1-3 nm, lateral dimension
10-20 μm, crystal structure is complete, is detailed in attached drawing 1a, and 1b, graphene microchip is soft, transparent, and crystal form keeps good, and electricity, heat pass
It is defeated to have excellent performance.
1 mass parts graphene powder is taken to be scattered in 10 mass parts water, mechanical stirring forms dispersion liquid, and 10 mass parts are added
Water-based acrylic resin lotion (resin), 0.2 mass parts carbon nanotube, 0.3 mass parts conductive black, 1 mass parts barium carbonate base
Ceramic PTC powder (self limiting temperature filler), 0.1 mass parts titanium dioxide (functional filler), 0.1 mass parts dodecyl benzene sulfonic acid
Sodium (dispersing agent), the polyether-modified polydisiloxane of 0.05 mass parts (defoaming levelling agent), stirring is sanded after 1 hour, is finally sieved
300 mesh obtain homogeneous graphene electric heating slurry.
Selection high-density plate is wood substrate, mechanical grinding is carried out to substrate surface, using the water of above-mentioned graphene powder
Dispersion liquid carries out spray treatment to substrate, and dispersion liquid concentration is 5 mg/mL, after dry 180 minutes under 60 °C, such as attached drawing 2b
It is shown.Each surface of wood substrate is coated with graphene, for enhancing each interlayer heat transfer.Obtained electric heating slurry is taken
Spraying method be compound in surface of wooden substrate formed network structure, after in closed oven drying, obtain conductive heating layer thickness
It is 20 μm, resistivity is about 0.2 Ω cm.30 μ m thick copper-foil conducting electricities are laid with, and is hit exactly in electric hot plate and places temperature sensing
Device.Take spraying technology in surface spraying polyurethane protective layer, protective layer thickness is 30 μm.This electric heating floor system wearing layer
To add aluminum oxide resin, decorative layer is melamine facing paper, and heat preservation reflecting layer is flame retardant type molded polystyrene bubble
Foam plate (EPS), as depicted in figure 2, the floor system successively includes wearing layer, dress to each layer mutual alignment relation from top to bottom
Adorn layer, wood substrate layer, graphene-based conductive heating layer, protective layer, heat preservation reflecting layer.30 V of operating voltage, temperate zone work temperature
30 °C of degree.
Embodiment 2
Graphene powder material is prepared using electrochemistry swelling graphite electrode method, graphene is with a thickness of 3-5 nm, lateral dimension
About 30-50 μm, crystal structure is complete, and graphene microchip is soft, transparent, and crystal form keeps good.
10 mass parts graphene powders are taken to be scattered in 200 mass parts water, mechanical stirring forms dispersion liquid, and 50 mass are added
Part water-based acrylic resin lotion (resin), 2 mass parts carbon nanotubes, 3 mass parts conductive blacks, 10 mass parts barium carbonate bases pottery
Porcelain PTC powder (self limiting temperature filler), 5 mass parts are without photocatalyst (functional filler), 0.3 mass parts neopelex
(dispersing agent), the polyether-modified polydisiloxane of 0.2 mass parts (defoaming levelling agent), stirring are sanded after 3 hours, are finally sieved 400
Mesh obtains homogeneous graphene electric heating slurry.
Selection high density fiberboard is wood substrate, sided corona treatment is taken to substrate surface, using above-mentioned graphene powder
Aqueous dispersions spray treatment is carried out to substrate, dispersion liquid concentration is 10 mg/mL, after dry 120 minutes under 100 °C.It will
Obtained electric heating slurry takes spraying method to be compound in surface of wooden substrate and forms network structure, after in closed oven drying,
Conductive heating layer is obtained with a thickness of 10 μm, resistivity is about 2 Ω cm.20 μ m thick conductive copper pastes are printed, and in electric hot plate
Place temperature sensor in center.Take spraying technology in surface spraying polyurethane protective layer, protective layer thickness is 30 μm.This electricity
Heating floor system wearing layer is addition aluminum oxide resin, and decorative layer is melamine facing paper, and heat preservation reflecting layer is to be laid with
There is the extruded sheet of aluminium foil.60 V of operating voltage, 45 °C of temperate zone operating temperature, when work, entire wood floors heating surface is uniform,
It is found after carrying out infrared imaging detection, cross-section fever in floor shows that heat can be transmitted from cross-section, it was demonstrated that wood substrate
Each surface is graphene coated can effectively to enhance each surface heat transfer.
Embodiment 3
Graphene powder material is prepared using electrochemistry swelling graphite electrode method, graphene is with a thickness of 1-5 nm, lateral dimension
About 50-100 μm, crystal structure is complete, and graphene microchip is soft, transparent, and crystal form keeps good.
It takes 20 mass parts graphene powder ultrasonic disperses in 500 mass parts ethyl alcohol, forms dispersion liquid, 50 mass parts are added
Aqueous polyurethane resin emulsion (resin), 3 mass parts carbon nanotubes, 5 mass parts conductive blacks, 20 mass parts carbonic acid barium-based ceramics
PTC powder (self limiting temperature filler), 1 mass parts magnesium hydroxide (functional filler), 0.5 mass parts neopelex (point
Powder), the polyether-modified polydisiloxane of 0.5 mass parts (defoaming levelling agent), stirring is sanded after 3 hours, and be finally sieved 300 mesh,
Obtain homogeneous graphene electric heating slurry.
Selection solid wood board is wood substrate, plasma cleaning is taken to substrate surface, using the water of above-mentioned graphene powder
Dispersion liquid carries out spray treatment to substrate, and dispersion liquid concentration is 15 mg/mL, after dry 60 minutes under 120 °C.It will obtain
Electric heating slurry take roll marks mode be compound in surface of wooden substrate formed dentalation, after in closed oven drying, obtain
For conductive heating layer with a thickness of 30 μm, resistivity is about 2 Ω cm.It is laid with 35 μ m thick copper-foil conducting electricities and conductive silver paste, and
Place temperature sensor in electric hot plate center.Spraying technology is taken to spray polyimide covercoat, protective layer thickness 30 on surface
μm.This electric heating floor system wearing layer is addition aluminum oxide overlay paper impregnated melamine resin, and decorative layer is facing paper,
Keeping the temperature reflecting layer is the polyethylene board for being equipped with aluminium foil.120 V of operating voltage, 50 °C of temperate zone operating temperature.
Embodiment 4
By graphite raw ore through broken, micro crystal graphite original ore powder or not sufficiently delaminated raw ore are made into electrode, made electrode by sieving
The electrolytic preparation graphene powder in electrolytic cell, for graphene with a thickness of 3-5 nm, lateral dimension is about 0.5-3 μm, is detailed in attached
Fig. 1 c, 1d, crystal structure is complete, and crystal form keeps good, may be constructed electric heating transport layer.
10 mass parts graphene powders are taken to be scattered in 300 mass parts water, mechanical stirring forms dispersion liquid, and 50 mass are added
The aqueous polymethyl methacrylate (resin) of part, 1 mass parts carbon nanotube, 3 mass parts conductive blacks, 3 mass parts electrically conductive graphites,
10 mass parts barium carbonate base ceramic PTC powder (self limiting temperature filler), 0.5 mass parts titanium dioxide (functional filler), 0.5 mass
Part neopelex (dispersing agent), the polyether-modified polydisiloxane of 0.2 mass parts (defoaming levelling agent), is stirred 2 hours
2 hours ball millings are carried out afterwards, are sanded within latter 1 hour, be finally sieved 400 mesh, obtains homogeneous graphene electric heating slurry.
Selection solid wood board is wood substrate, surface mechanical grinding is taken to substrate surface, using above-mentioned graphene powder
Aqueous dispersions carry out spray treatment to substrate, and dispersion liquid concentration is 20 mg/mL, after dry 100 minutes under 120 °C.Will
To electric heating slurry take mode of printing to be compound in surface of wooden substrate to form dentalation, after it is dry in infrared light irradiation, obtain
To conductive heating layer with a thickness of 40 μm, resistivity is about 20 Ω cm.It is laid with 35 μ m thick copper-foil conducting electricities and conductive silver paste,
And it is hit exactly in electric hot plate and places temperature sensor.Doctor blade technique is taken to scratch protective polyurethane layer on surface, protective layer thickness is
20 μm.This electric heating floor system wearing layer is addition aluminum oxide overlay paper impregnated melamine resin, and decorative layer is decoration
Paper, heat preservation reflecting layer is the polystyrene foam plate for being equipped with aluminium foil.220 V of operating voltage, 65 °C of temperate zone operating temperature.
Embodiment 5
By graphite raw ore through broken, micro crystal graphite original ore powder or not sufficiently delaminated raw ore are made into electrode, made electrode by sieving
The electrolytic preparation graphene powder in electrolytic cell, graphene is with a thickness of 1-5 nm, and lateral dimension is about 1-3 μm, crystal structure
Completely, crystal form keeps good.
It takes 20 mass parts graphene powder ultrasonic disperses in 400 mass parts ethyl alcohol, forms dispersion liquid, 40 mass parts are added
Aqueous melamine formaldehyde resin (resin), 0.5 mass parts carbon nanotube, 2 mass parts conductive blacks, 2 mass parts electrically conductive graphites,
20 mass parts boronation titanium-based PTC(self limiting temperature fillers), 1 mass parts zinc oxide (functional filler), 0.3 mass parts coke grace acid sodium
(dispersing agent), 0.2 mass parts fluoro-acrylate copolymer (defoaming levelling agent), stirring carry out 1 hour ball milling after 1 hour, and rear 3
Hour is sanded, and be finally sieved 300 mesh, obtains homogeneous graphene electric heating slurry.
Selection high-density plate is wood substrate, surface mechanical grinding is taken to substrate surface, using above-mentioned graphene powder
Aqueous dispersions spray treatment is carried out to substrate, dispersion liquid concentration is 30 mg/mL, after dry 120 minutes under 100 °C.It will
Obtained electric heating slurry takes spraying method to be compound in surface of wooden substrate and forms dentalation, after it is dry in thermal convection, obtain
For conductive heating layer with a thickness of 50 μm, resistivity is about 2 Ω cm.It is laid with 45 μ m thick copper-foil conducting electricities and conductive silver paste, and
Place temperature sensor in electric hot plate center.Doctor blade technique is taken to scratch ABS resin protective layer, protective layer thickness 20 on surface
μm.This electric heating floor system wearing layer is addition aluminum oxide overlay paper impregnated melamine resin, and decorative layer is facing paper,
Keeping the temperature reflecting layer is the extruded sheet for being equipped with aluminium foil.110 V of operating voltage, 50 °C of temperate zone operating temperature.
Embodiment 6
Graphene powder material is prepared using electrochemistry swelling graphite electrode method, graphene is with a thickness of 0.5-5 nm, lateral ruler
Very little about 50-100 μm, crystal structure is complete, and graphene microchip is soft, transparent, and crystal form keeps good.
It takes 5 mass parts graphene powder ultrasounds, be dispersed with stirring in 20 mass parts acetone, mechanical stirring forms dispersion liquid, adds
Enter 10 mass parts polymethyl methacrylates (resin), 0.1 mass parts carbon nanotube, 1 mass parts conductive black, 1 mass parts lead
Electro-graphitic, 1 mass parts barium carbonate base ceramic PTC powder (self limiting temperature filler), 0.1 mass parts magnesium hydroxide (functional filler),
0.5 NONIN HS 240 (dispersing agent), 0.1 polyether modified silicon oil (defoaming levelling agent), stirring is sanded after 3 hours, most
After be sieved 300 mesh, obtain homogeneous graphene electric heating slurry.
Selection medium-density plate is wood substrate, mechanical grinding is carried out to substrate surface, using the water of above-mentioned graphene powder
Dispersion liquid carries out spray treatment to substrate, and dispersion liquid concentration is 20 mg/mL, after dry 100 minutes under 100 °C.It will obtain
Electric heating slurry take spraying method to be compound in surface of wooden substrate to form dentalation, after it is dry in infrared light irradiation, obtain
For conductive heating layer with a thickness of 30 μm, resistivity is about 40 Ω cm.35 μ m thick conducting aluminum pastes and conductive silver paste are sprayed,
Middle conductive silver paste is directly contacted with graphene heating layer, and conductive copper paste is contacted with conductive silver paste again, and at edge and in electric hot plate
Place temperature sensor in center.Doctor blade technique is taken to spray protective polyamide layer on surface, protective layer thickness is 30 μm.This electricity
Heating floor system wearing layer is addition aluminum oxide resin, and decorative layer is decoration veneer, and heat preservation reflecting layer is extruded sheet.Work
Make 120 V of voltage, 65 °C of temperate zone operating temperature.
Embodiment 7
By graphite raw ore through broken, micro crystal graphite original ore powder or not sufficiently delaminated raw ore are made into electrode, made electrode by sieving
The electrolytic preparation graphene powder in electrolytic cell, graphene is with a thickness of 3-5 nm, and lateral dimension is about 1-3 μm, crystal structure
Completely, crystal form keeps good.
15 mass parts graphene powders are taken to be dispersed with stirring in 500 mass parts propylene glycol ether solvents, mechanical stirring, which is formed, divides
25 mass parts aqueous polyurethane resin emulsions (resin), 1 mass parts carbon nanotube, 3 mass parts conductive blacks, 5 matter are added in dispersion liquid
Measure part electrically conductive graphite, 10 mass parts barium carbonate base ceramic PTC powder (self limiting temperature filler), 0.5 mass parts dodecyl benzene sulfonic acid
Sodium (dispersing agent), 0.5 mass parts aluminum stearate (defoaming levelling agent), stirring is sanded after 2 hours, and be finally sieved 400 mesh, obtains
Matter graphene electric heating slurry.
Selection solid wood board is wood substrate, plasma cleaning processing is carried out to substrate surface, using above-mentioned graphene powder
Aqueous dispersions spray treatment is carried out to substrate, dispersion liquid concentration is 50 mg/mL, after dry 90 minutes under 120 °C.Will
To electric heating slurry take mode of printing to be compound in surface of wooden substrate to form dentalation, after it is dry in infrared light irradiation, obtain
To conductive heating layer with a thickness of 50 μm, resistivity is about 100 Ω cm.10 μm of conductive silver pastes of printing in advance, re-lay 35
μ m thick copper-foil conducting electricity, wherein conductive silver paste is directly contacted with graphene heating layer, and copper-foil conducting electricity is contacted with conductive silver paste again, and
Placement temperature sensor is hit exactly at edge and in electric hot plate.It takes printing technology to spray polyetherimide protective layer on surface, protects
Covering thickness is 100 μm.This electric heating floor system wearing layer is addition aluminum oxide resin, and decorative layer is melamine dress
Paper is adornd, heat preservation reflecting layer is polyethylene board.220 V of operating voltage, 55 °C of temperate zone operating temperature.
Claims (10)
1. a kind of graphene-based self limiting temperature electric heating slurry, it is characterised in that: the raw material including following weight proportion:
Graphene: 1-20 parts,
Dispersion liquid solvent: 10-500 parts,
Resin: 10-50 parts,
Electric heating filler: 0.5-10 parts,
Self limiting temperature PTC filler: 1-20 parts,
Functional stuffing: 0-5 parts,
Dispersing agent: 0-0.5 parts,
Defoaming levelling agent: 0-0.5 parts；
Above-mentioned raw materials prepare graphene-based self limiting temperature electric heating slurry after being mixed.
2. graphene-based self limiting temperature electric heating slurry according to claim 1, it is characterised in that: the graphene be powder or
Liquid slurry；Graphene microchip contains one or more of hydroxyl, carboxyl, amino, nitro functions；Graphene thickness < 5
Nm, 0.5~100 μm of lateral dimension, crystal structure is complete；
Dispersion liquid solvent used includes one of water, alcohol solvent, ketone solvent, alcohol ethers solvent；
The resin includes water-based acrylic resin lotion, aqueous polyurethane resin emulsion, polymethyl methacrylate, melamine
One of amine-formaldehyde resins；
The electric heating filler includes the mixture of one or more of carbon nanotube, conductive black, electrically conductive graphite；
The self limiting temperature PTC filler includes one of barium carbonate base ceramic PTC, boronation titanium-based PTC, polymer resin base PTC；
It is 0.5-10 μm that self limiting temperature PTC filler, which is through one of ball milling, sand milling or spray drying or the obtained partial size of any combination,
Filler particles；
The functional stuffing includes the mixture except one or more of formaldehyde filler, fire-retardant filler, infrared reinforcing filler；
The formaldehyde filler that removes includes cold catalyst, MHCC material, without one of photocatalyst, and MHCC material is to select high-specific surface area
Active material is substrate, the efficient catalyst made from microwave treatment after active liquid dipping；Fire-retardant filler includes magnesium hydroxide, hydrogen-oxygen
Change one of aluminium；Infrared reinforcing filler includes one of zirconium oxide, zinc oxide；
The dispersing agent includes neopelex, polyalcohol, neopelex, burnt grace acid sodium, polyoxy second
One of alkene octyl phenyl ether, carboxymethyl cellulose；
The defoaming levelling agent includes polyether modified silicon oil, fluoro-acrylate copolymer, polyether-modified polydisiloxane, hard
One of fatty acid amide, aluminum stearate.
3. a kind of preparation method of graphene-based self limiting temperature electric heating slurry of any of claims 1 or 2, it is characterised in that: including
Following steps:
(a) graphene powder or dispersions in liquids for choosing different sizes, thickness, carry out pre-dispersed；
(b) resin, electric heating filler, self limiting temperature PTC filler, functional stuffing, dispersing agent, defoaming levelling agent are added and is stirred in proportion
It mixes, after being dispersed with stirring 1-3h, carries out grinding 0.5h ~ 6h, after being ground to granularity less than 50 microns, homogenous disperse liquid is obtained, to this
Homogenous disperse liquid carries out sieving processing, removes remaining reunion graphene and undissolved auxiliary agent on sieve, be made it is graphene-based from
Limit warm electric heating slurry.
4. the preparation method of graphene-based self limiting temperature electric heating slurry according to claim 3, it is characterised in that: step a) institute
That states is pre-dispersed using ultrasonic disperse or mechanical stirring composite diffusion mode；Lapping mode used in step b) include mechanical ball mill,
One of sand mill grinding, three-roll grinder grinding or any combination；The sieve mesh number of the sieving processing is 300-400
Mesh can remove residual bulky grain insoluble matter on sieve.
5. a kind of application of graphene-based self limiting temperature electric heating slurry of any of claims 1 or 2 in electric heating floor system.
6. application according to claim 5, it is characterised in that: electric heating is made using graphene-based self limiting temperature electric heating slurry
Plate, the floor system successively include wearing layer, decorative layer, substrate layer, graphene-based conductive heating layer, protection from top to bottom
Layer, heat preservation reflecting layer.
7. application according to claim 6, it is characterised in that: steps are as follows for the preparation process of electric heating floor:
(1) wood substrate is surface-treated；
(2) each surface of wood substrate is covered into pure graphite ene coatings；
(3) drying and processing；
(4) graphene-based electric heating slurry is carried out being compounded to form graphene conductive fever with the wood substrate for being coated with pure graphene
Layer；
(5) it is dried；
(6) conductive metal lines are laid with and install temperature control sensor；
(7) armor coated.
8. application according to claim 7, it is characterised in that: the following steps are included:
(1) wood substrate is surface-treated；The surface treatment refers to using mechanical surface polishing, plasma technique
Or sided corona treatment method improves surface of wooden substrate active force, strengthening slurry binding force；
(2) six surfaces of cuboid wood substrate are covered into pure graphite ene coatings；
The graphite ene coatings refer to pure graphene aqueous liquid dispersion, and the concentration of pure graphene aqueous liquid dispersion is 5 mg/mL
– 50 mg/mL；The surface covering, which refers to, coats graphene coating uniform using the technique in spraying, being immersed in；
(3) drying and processing, no less than 60 minutes are carried out under 60-120 °C；
(4) graphene-based electric heating slurry is subjected to combination process with the wood substrate for being coated with pure graphene, forms graphene and leads
Electric heating layer；The shape of conductive heating layer is latticed or dentation；Conductive heating layer with a thickness of 5-50 μm；Resistivity value is 0
.2-200 Ω·cm；
Compound includes one of printing, roll marks, spraying process；
(5) it is dried: one of dry using closed oven drying, the drying of infrared light irradiation, thermal convection drying, UV；
(6) conductive metal lines are laid with and install temperature control sensor；Temperature control sensor includes temperature sensor and overheat protector；
Conductive metal includes the combination of one or more of copper-foil conducting electricity, conductive copper paste, conducting aluminum paste and conductive silver paste；Conductive gold
The thickness of the thickness and electric heating slurry that belong to track laying is close, and the two thickness difference is at ± 10 μm；
(7) armor coated: protective layer is in polyurethane, ABS resin, polyamide, polysulfones, polyimides or polyetherimide
One kind, coating processes include printing, blade coating, spraying one of, coating thickness be 0.03-0.3 mm.
9. application according to claim 6, it is characterised in that:
The wearing layer is by addition aluminum oxide resin or addition aluminum oxide overlay paper impregnated melamine resin group
At；
The decorative layer is one of melamine facing paper, PVC, decoration veneer；
The substrate layer is one of high-density plate, medium-density plate, particieboard, solid wood board；
The heat preservation reflecting layer is one of flame retardant type molded polystyrene foams plate, extruded sheet, polyethylene board；Heat preservation
Layer is equipped with aluminium foil reflecting layer close to protective layer side.
10. application according to claim 6, it is characterised in that: the electric heating operating voltage of electric heating floor is 10-220 V；
Steady state operating temperature is 30-95 °C.
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| CN111876027A (en) * | 2020-05-23 | 2020-11-03 | 广东日禾电器有限公司 | Preparation method of self-temperature-limiting heating coating material |
| CN112360088A (en) * | 2020-10-12 | 2021-02-12 | 南京顺天智能科技有限公司 | Air heat-preservation self-heating floor and manufacturing method thereof |
| CN112406232A (en) * | 2020-11-12 | 2021-02-26 | 青岛德通纳米技术有限公司 | Ultraviolet aging resistant graphene wood-plastic floor and manufacturing method thereof |
| CN112593415A (en) * | 2020-12-01 | 2021-04-02 | 肃宁县中原纺织有限责任公司 | Water-based graphene flame-retardant PTC conductive paste, preparation method thereof and flexible conductive heating cloth |
| CN112893059A (en) * | 2021-01-22 | 2021-06-04 | 江苏江南烯元石墨烯科技有限公司 | Method for enhancing adhesion between graphene heating coating and substrate |
| CN113621273A (en) * | 2021-10-13 | 2021-11-09 | 广东简一(集团)陶瓷有限公司 | Self-temperature-limiting conductive ink, preparation method and heating ceramic |
| CN113621273B (en) * | 2021-10-13 | 2022-01-11 | 清远市简一陶瓷有限公司 | Self-temperature-limiting conductive ink, preparation method and heating ceramic |
| CN114621611A (en) * | 2022-04-02 | 2022-06-14 | 北京斯年智驾科技有限公司 | Heating material with graphene sprayed on ceramic surface |
| CN115910428A (en) * | 2022-12-01 | 2023-04-04 | 深圳清研装备科技有限公司 | Preparation method and application of carbon-based composite conductive particles |
| CN115910428B (en) * | 2022-12-01 | 2024-05-31 | 深圳清研锂业科技有限公司 | Preparation method and application of carbon-based composite conductive particles |
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Application publication date: 20190405 |