CN107995704A - Electric heating film that a kind of graphene oxide is modified and its preparation method and application - Google Patents
Electric heating film that a kind of graphene oxide is modified and its preparation method and application Download PDFInfo
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- CN107995704A CN107995704A CN201711308282.1A CN201711308282A CN107995704A CN 107995704 A CN107995704 A CN 107995704A CN 201711308282 A CN201711308282 A CN 201711308282A CN 107995704 A CN107995704 A CN 107995704A
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- graphene oxide
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- crosslinking agent
- electric heating
- heating film
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- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 90
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- 238000002360 preparation method Methods 0.000 title claims abstract description 21
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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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/04—Coating
- C08J7/0427—Coating with only one layer of a composition containing a polymer binder
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/12—Chemical modification
- C08J7/123—Treatment by wave energy or particle radiation
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2379/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen, or carbon only, not provided for in groups C08J2361/00 - C08J2377/00
- C08J2379/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
- C08J2379/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2433/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
- C08J2433/04—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters
- C08J2433/06—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters of esters containing only carbon, hydrogen, and oxygen, the oxygen atom being present only as part of the carboxyl radical
- C08J2433/08—Homopolymers or copolymers of acrylic acid esters
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2463/00—Characterised by the use of epoxy resins; Derivatives of epoxy resins
- C08J2463/04—Epoxynovolacs
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
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- Chemical & Material Sciences (AREA)
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- Chemical Kinetics & Catalysis (AREA)
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- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Conductive Materials (AREA)
Abstract
Electric heating film being modified the present invention provides a kind of graphene oxide and its preparation method and application.A kind of preparation method for the electric heating film that graphene oxide is modified, the electric heating film include stacked conductive layer and heating layer；The heating layer is the layer that the ink containing graphene oxide is formed by irradiation；The ink containing graphene oxide includes at least graphene oxide, water, free radical scavenger and resinoid bond.The preparation method of the present invention need not introduce the larger chemical reducing agent of toxicity, curing agent, and without pretreatment, therefore, this method has the advantages that environmental protection, technique is simple, production efficiency is high.
Description
Technical field
The present invention relates to chemical field, the electric heating film being modified more particularly, to a kind of graphene oxide and preparation method thereof
And application.
Background technology
The principle of traditional electric heating film is that heating area is small by resistance wire electrified regulation, and electrothermal efficiency is low, resistance filament length
Time easily aoxidizes, and security is low, short life.Therefore need to find a kind of good mode of heating of security to substitute traditional add
Hot mode, to meet the life requirement of people.
Graphene is with SP by carbon atom2The monoatomic layer of hybrid form connection is formed, and is presently found known materials
In most thin most rigid material.The special structure of graphene makes it contain many unique physics and chemical property, makes
It makes it have huge application in electronics or even heating art with excellent conduction, heat conductivility, these excellent performances
Value.
In the prior art, patent application CN104219797A discloses a kind of preparation method of graphene Electric radiant Heating Film：It is first
First using graphene oxide film forming after, then it is reduced, reduction process uses substantial amounts of chemical reducing agent, and toxicity compared with
Greatly, operating procedure is complicated.Patent application CN105906832A discloses a kind of preparation method of graphene water-based electric heating film：Due to
Inert condition is presented in graphene surface, weak with the interaction of other media, and there are stronger model between graphene film and piece
De Huali, easily reunites, it is difficult to dispersed in fibrous inside or surface, it is impossible to which the excellent performance of graphene is fully protected
Stay in the composite, thus the invention first to graphene carry out hydrophily processing, add solution of cellulose derivative into
Row is pre-dispersed, although reducing the use of chemical reagent, graphene is pre-processed, and operating procedure is complicated.
In view of this, it is special to propose the present invention.
The content of the invention
A kind of preparation method for the electric heating film being modified it is a primary object of the present invention to provide graphene oxide, it is described
Preparation method need not introduce the larger chemical reducing agent of toxicity, curing agent, and without pretreatment, therefore, this method has
Environmental protection, the advantages that technique is simple, production efficiency is high.
In order to realize the above object the present invention provides following technical scheme：
A kind of preparation method for the electric heating film that graphene oxide is modified, the electric heating film include stacked conductive layer and
Heating layer；
The heating layer is the layer that the ink containing graphene oxide is formed by irradiation；
The ink containing graphene oxide includes at least graphene oxide, water, free radical scavenger and resinoid bond.
The method made above of the present invention improves technique from following several respects, improves properties of product：
First, graphene is replaced using graphene oxide, so that the step of eliminating graphene pretreatment, simplifies technique,
Improve production efficiency.
2nd, existing electronation is instead of by the way of redox graphene is irradiated, is asked so as to solve pollution
Topic.Specifically, irradiation can make water power separate out H free radicals, aqueous electron e- aqWith OH free radicals, H free radicals and hydration electricity
Son has very strong reduction, and graphene oxide is reduced to graphene using H free radicals and aqueous electron, is recycled certainly
OH free radicals are removed by base agent for capturing.
3rd, the ink that graphene oxide and resinoid bond are formed can form the film for stablizing, having certain mechanical strength,
Not just for simple physical mixed, some graphene oxide between graphene oxide and resinoid bond in the present invention
With resinoid bond by irradiation post-crosslinking to together, crosslinking between the two not only improves graphene oxide on heating layer
The uniformity of distribution, and improve film strength.
4th, the heat dissipation performance that graphene oxide improves electric heating film is introduced, and then improves the utilization efficiency of heat energy of Electric radiant Heating Film.
5th, by the way of radiation curing, ink solidification is formed a film, without using curing agent, reduces raw materials consumption, is dropped
Low production cost.
In conclusion the present invention, which not only solves, adds technical problem existing for graphene in existing Electric radiant Heating Film, but also
The heat conductivility of electric heating film can be improved, while other performance is at least up to the level equal with existing product.
Raw material used in the present invention --- graphene oxide refers to graphene oxide made from any means, and (name definition is joined
See graphene alliance standard T/CGIA 001-2017).
Method made above can also be improved from the following aspect, specific as follows.
Preferably, the dosage rate of the irradiation is 1-600KGy/h, it is preferred to use cobalt -60 (60Co) gamma-ray radiation source or
Electron accelerator carries out the irradiation.
Irradiation dose to the distribution on heating layer of the reducing degree, GO of graphene oxide (GO) and GO with it is resin-bonded
Bonding strength between agent has a major impact, and through screening, convenient irradiation dose is 1-600KGy/h, more preferably 100-
300KGy/h, for example, 1KGy/h, 10KGy/h, 20KGy/h, 50KGy/h, 100KGy/h, 150KGy/h, 200KGy/h,
250KGy/h, 300KGy/h, 350KGy/h, 400KGy/h, 450KGy/h, 500KGy/h, 550KGy/h, 600KGy/h etc..
During practical operation, possibly constant irradiation dose can not be realized, it is allowed to have a certain range of fluctuation.
The radiation source usually irradiated does not limit, such as common -60 (60Co) gamma-ray radiation source or electron accelerator,
Or the αsource of caesium -137, Iridium-192 source, gamma ray radiator etc., preferably -60 (60Co) gamma-ray radiation source or electron accelerator.
Preferably, in the ink containing graphene oxide, the concentration of graphene oxide is 1%-15%, preferably 5%-
10%；Heretofore described concentration " % " refers to the weight g of solute contained in every 100mL solution.
Preferably, in the ink of the graphene oxide, the weight ratio of water and free radical scavenger is 1-10:1.
Microstructure and macrostructure of the weight ratio of the concentration of graphene oxide, water and free radical scavenger to heating layer
All have an impact, therefore reflect onto product, not only have an impact to the thermal conductivity of Electric radiant Heating Film, also have an impact on other influences.To obtain
Preferable comprehensive performance, the concentration of graphene oxide are preferably 1%-15%, such as 1%, 5%, 7%, 9%, 10%,
13%th, 15% etc.；The weight ratio of water and free radical scavenger is 1:1、2:1、3:1、4:1、5:1、6:1、7:1、8:1、9:1、10:
1 etc..
Preferably, in the ink containing graphene oxide, the weight ratio of graphene oxide and resinoid bond is 1:3-
12.Matching somebody with somebody between graphene oxide and resinoid bond compares the film forming of ink and the electric conductivity of Electric radiant Heating Film has an impact, through examining
Examine, both preferable weight ratios are 1:3-12, such as 1:3、1:4、1:5、1:6、1:7、1:8、1:9、1:10、1:11、1:12 etc..
Preferably, the free radical scavenger is the one or more in alcohol, amine and ketone；The alcohol be preferably selected from methanol,
One or more in ethanol and isopropanol；Such as alcohol, amine, ketone, the mixing of alcohol and amine, the mixing of alcohol and ketone, or amine and ketone
Mixing, or the mixing of alcohol, amine and ketone three.
Wherein, the alcohol is preferably selected from the one or more in methanol, ethanol and isopropanol；Such as methanol, ethanol, isopropyl
The mixing of the mixing of the mixing of alcohol, methanol and ethanol, methanol and isopropanol, ethanol and isopropanol, or methanol, ethanol and isopropanol
The mixing of three.In above scheme, preferred isopropanol.
The amine is preferably selected from the one or more in monoethanolamine, diethanol amine and triethanolamine, such as monoethanolamine, diethyl
The mixing of the mixing of hydramine, triethanolamine, monoethanolamine and diethanol amine, monoethanolamine and triethanolamine, monoethanolamine, diethanol amine and
The mixing of triethanolamine three；In above scheme, preferred triethanolamine.
The ketone is the mixing of acetone or butanone or both.
Preferably, the resinoid bond is the one or more in epoxy resin, acrylic resin and organic siliconresin,
Preferred epoxy.
Through investigating, when selecting epoxy resin as binding agent, the mechanical strength of film can not only be improved, and can improve
Graphene and cross-linkage of resin.In addition, it can arbitrarily select the type of epoxy resin.
Preferably, the ink is also comprising at least one of photoinitiator, crosslinking agent and diluent, such as only add light
Initiator, or crosslinking agent is only added, or diluent is only added, or photoinitiator and crosslinking agent are added at the same time, or light is added at the same time
Initiator and diluent, or diluent and crosslinking agent are added at the same time, or photoinitiator, crosslinking agent and diluent are added at the same time.
Radiation curing is using high energy electron bombardment ink molecules, is broken its double bond, resolves into free radical or ion, from
And trigger the double-bond polymerization of system to react, film-forming.Radiation curing technology is an energy saving and new technology for environment-friendly type, it is complete
Meet " 3E principles " entirely, radiation curing technique not only can guarantee that coating layer thickness, and have excellent performance, and reduces raw material and disappear
Consumption, advantageously reduces financial cost.Specific radiation curing mode is related to the type of resinoid bond, and most of resin occurs
Cationic polymerization occurs for radical polymerization, small part, also has small part that radical polymerization had not only occurred but also cationic polymerization occurs, because
This can choose whether to add photoinitiator in actual fabrication process according to the type of resin.
Diluent is mainly used for adjusting the viscosity of ink, to match corresponding film-forming process (coating, printing, impregnating).
Crosslinking agent can increase the cross-linking amount and crosslinked stability between graphene oxide and fibre-forming polymer.Crosslinking
On the one hand agent is inserted into the lamellar structure of graphene oxide as the bridge formation between graphene oxide and resin, makes oxidation stone
Black alkene can keep good characteristic while being inserted into molecular resin, graphene oxide is reticulated knot with resin crosslinks
Structure, had not only retained the good characteristic of resin, but also improved the bond strength between graphene oxide and resin.It is excellent based on object above
Select the one or more in alkenes crosslinking agent, organic silicon crosslinking agent and epichlorohydrin resin class crosslinking agent, these crosslinking agents
It can realize object above, and obtain preferable effect.These crosslinking agents can be used alone, and can also be combined makes
With, such as alkenes crosslinking agent and organic silicon crosslinker combination, or organic silicon crosslinking agent and the friendship of epichlorohydrin resin class
Join agent combination, either alkenes crosslinking agent is handed over epichlorohydrin resin class crosslinker combination or alkenes crosslinking agent, organic silicon
Join agent and epichlorohydrin resin class crosslinking agent three combination, preferable resultant effect can be obtained when being applied in combination.
Preferably, the alkenes crosslinking agent is selected from polyethyleneglycol diacrylate, polyethylene polyamine, three allyl of melamine
One or more in ester, triallyl cyanurate, trimethylolpropane tris-(3- aziridinyls)-propionic ester.
Polyethyleneglycol diacrylate, polyethylene polyamine, melamine triallyl, triallyl cyanurate, three hydroxyls
Methylpropane three-(3- aziridinyls)-propionic ester has stronger conjugation, and the cross-linking system formed is more stable.
Preferably, the organic silicon crosslinking agent is silane coupling agent.
Silane coupling agent can not only the stability that combines of reinforced resin and graphene oxide, but also ink can be improved
Film forming.In principle, arbitrary silane coupling agent YSiX3It is all feasible, n=0~3；X is hydrolyzable group, be typically chloro,
Methoxyl group, ethyoxyl, methoxy ethoxy, acetoxyl group etc., generate silanol (Si (OH) when these groups hydrolyze3), and with
Inorganic substances combine, and form siloxanes；Y is organo-functional group, can be reacted with resin, is vinyl, amino, epoxy group, first
Base acryloxy, sulfydryl or urea groups.In above type, vinyl silanes, amino silane, epoxy radicals silicone hydride, mercapto can be selected
Base silane and methacryloxypropyl silane etc., these crosslinking agents can be used alone, and also can be combined and use, wherein optimal ethylene
Base.
Preferably, the epichlorohydrin resin class crosslinking agent is crosslinking agent DE, crosslinking agent EH, crosslinking agent FH etc..
The advantages of epichlorohydrin resin class crosslinking agent is that dissolubility is good, and use condition is gentle, and DE, EH and FH can individually make
With can also be applied in combination, preferably individually use crosslinking agent DE.
Furthermore it is preferred that the photoinitiator includes diazol, diaryl group iodized salt, triaryl sulfonium salts, alkyl sulfosalt, iron
One or more mixing in arene salt, sulfonyloxy ketone and triaryl silica ether, preferably diaryl group iodized salt.
Preferably, the diluent is TMPTA, TPGDA, HDDA, DPGDA, EO-TMPTA, alkyl glycidyl ether, second
One or more in glycol glycidol ether, trimethylolpropane glycidol ether, toluene glycidol ether.These diluents
The viscosity of ink system can not only be adjusted, and is played the role of to filming performance important.
Arbitrary conductive material or electrode can be selected in the conductive layer of the present invention.
Preferably, the conductive layer includes silver electrode layer and copper electrode layer；The size of electrode layer is adjusted according to purposes, such as
Printed electrode bar with conductive silver paste, printing width 8-20mm, preferably 8-15mm, 8-30 μm of thickness, preferably 10-15 μm, silver paste electricity
Copper foil electrode layer is covered on the layer of pole.
Preferably, the thickness of the heating layer is 8-30 μm, preferably 10-15 μm；
Preferably, the outer surface of the electric heating film is provided with insulating layer, is preferably provided with two layers up and down, improves security.
The material of insulating layer can be selected arbitrarily, such as the one or more in the polyester material such as PI, PVC, PE, PET, preferably PI；Insulation
The thickness of layer can set 10-50 μm, 20-25 μm of preferred thickness.
The electric heating film of the present invention can be arbitrary shape.
In the present invention, the laminating type between insulating layer, heating layer and conductive layer can use arbitrarily, such as dipping, painting
Cloth and printing etc..By taking printing as an example, the ink of intaglio printing (or silk-screen printing) containing graphene oxide on lower insulating layer, then
Irradiation (reactions such as reduction, crosslinking, curing occur for irradiation process), republishes conductive silver paste, covers copper foil electrode layer, afterwards afterwards
Upper insulating layer is covered on copper foil again, up to (can also hot repressing improve firmness).
The electric heating film being modified by the graphene oxide made of method made above of the present invention is widely used, available for making
Make the heating equipment in multiple industries such as construction industry, electronics industry, power industry and aerospace industry, the heating equipment bag
Include electric heating fabrics, heat conduction work clothes, electric heating bandage etc..
To sum up, compared with prior art, invention achieves following technique effect：
(1) add graphene oxide into the heating layer of electric heating film, using the mode redox graphene of irradiation, increase
The thermal diffusivity of electric heating film, and the level that other performances can at least reach and traditional electric heating film is equal are added, have added for tradition electricity
Hotting mask provides preferable substitute, it is thus also avoided that the problems such as traditional handicraft is complicated, of high cost.
(2) comprehensive performance of electric heating film is improved by increasing crosslinking agent.
(3) ink solidification is formed a film by the way of irradiation, reduces the use of curing agent, reduce disappearing for raw material
Consumption, reduces production cost, is a kind of efficient, economic, energy saving, environmental-friendly curing mode.
Embodiment
Technical scheme is clearly and completely described below in conjunction with embodiment, but ability
Field technique personnel will be understood that following described embodiment is part of the embodiment of the present invention, instead of all the embodiments,
The present invention is merely to illustrate, and is not construed as limiting the scope of the invention.Based on the embodiments of the present invention, the common skill in this area
Art personnel all other embodiments obtained without making creative work, belong to the model that the present invention protects
Enclose.The person that is not specified actual conditions in embodiment, the condition suggested according to normal condition or manufacturer carry out.Agents useful for same or instrument
Production firm person is not specified, is the conventional products that can be obtained by commercially available purchase.
The type for the graphene oxide composite material that following embodiments of the present invention are provided has：
Graphene oxide A：The graphene oxide prepared by Hummers methods.
Graphene oxide B：The graphene oxide prepared by Brodie methods.
Embodiment 1
The first step：The preparation of graphene oxide ink
Weigh 6 grams of graphene oxide, 3 grams of water, diluent (TMPTA) in right amount, 1 gram of NITRODIAZONIUM FLUOROBORATE, epoxy novolac tree
20 grams of fat (holy well SQAN-201, as binding agent), is uniformly mixed, then adds 3 grams of isopropanols thereto, is mixed equal
It is even, the graphene oxide ink containing isopropanol is obtained, wherein, the concentration of graphene oxide is 1%.
Second step：The printing of graphene oxide heating film
Using intaglio printing, the graphene oxide ink containing isopropanol is printed on Kapton.Printing
Thickness is 15 μm.Primary solidification obtains graphene oxide film.
3rd step：The irradiation of graphene oxide heating layer
Using cobalt -60 (60Co) gamma-ray radiation source, uses dosage rate as 300KGy/h, the oxidation stone that second step is obtained
Black alkene film irradiates 1h, and the film after irradiation is put in 160 DEG C of baking ovens dry 10min, obtains oxidation graphene film.
4th step：The encapsulation of heating layer.
Printed electrode at oxidation graphene film both ends with conductive silver paste after bar is dried and obtain silver electrode layer, printing width
10mm, 10 μm of thickness, copper foil electrode layer is covered on silver electrode layer, upper insulating layer is covered on copper foil, has been obtained after hot pressing
Whole electric heating film.
Embodiment 2-7
From embodiment 1 to differ only in irradiation dose different, be respectively：1KGy/h、10KGy/h、100KGy/h、
200KGy/h、400KGy/h、600KGy/h。
Embodiment 8-9
It is different from the addition for differing only in water in the first step of embodiment 1, be respectively：15 grams (embodiments 8), 30 grams
(embodiment 9).
Embodiment 10-11
It is different from the addition for differing only in resinoid bond of embodiment 1, respectively 30 grams (embodiments 10), 90 grams
(embodiment 11).
Embodiment 12-14
Difference from embodiment 1 is only different (being adjusted by the amount of diluent) in the concentration of graphene oxide, is respectively 5%
(embodiment 12), 10% (embodiment 13), 15% (embodiment 14).
Embodiment 15-16
It is different from the type for differing only in free radical scavenger of embodiment 1, the isopropanol of embodiment 1 is replaced respectively
For：Triethanolamine (embodiment 15), acetone (embodiment 16).
Embodiment 17
Differ only in that resinoid bond type is different, and binding agent is n-butyl acrylate resin from embodiment 1, also plus
Photoinitiator agent-diphenyl iodine hexafluorophosphate is entered.
Embodiment 18-19
Crosslinking agent is also added into the first step with differing only in for embodiment 1, crosslinking agent is respectively：Polyethylene glycol dipropyl
Olefin(e) acid ester (embodiment 18), crosslinking agent DE (embodiment 19), and the weight of crosslinking agent and graphene oxide in embodiment 18 to 19
Amount is than being all 1:1.
Embodiment 20
It is different from the type for differing only in graphene oxide of embodiment 1, graphene oxide A is replaced with into graphite oxide
Alkene B.
Comparative example 1
The first step：The preparation of ink
Weigh 6 grams of graphene, 20 grams of diluent (TMPTA), polyamide-based 1 gram of curing agent, epoxy adhesive (holy well
SQAN-201) 20 grams, 10 grams of modest 9250 dispersant of moral, is mixed evenly, obtains ink.
Second step：The printing of ink
Using intaglio printing, the ink containing graphene is printed on Kapton.The thickness of printing is 15 μm.
3rd step：Cure
Second step is obtained into film and is put in 160 DEG C of baking ovens dry 30min.
4th step：The encapsulation of heating layer.
Printed electrode at heating layer both ends with conductive silver paste after bar is dried and obtain silver electrode layer, printing width 10mm, 10 μ of thickness
M, copper foil electrode layer is covered on silver electrode layer, upper insulating layer is covered on copper foil, obtained after hot-press solidifying complete electricity plus
Hotting mask.
Performance test：
Film resistor Rs：Utilize four-point probe testing film resistance
Electric radiation transfer efficiency：Method carries out as defined in the 17th chapter in GB/T 7287-2008
The performance of electric heating film is as shown in table 1 obtained by all of above embodiment and comparative example.
1 graphene oxide of table is modified the performance of Electric radiant Heating Film
Finally it should be noted that：The above embodiments are only used to illustrate the technical solution of the present invention., rather than its limitations；To the greatest extent
Pipe is described in detail the present invention with reference to foregoing embodiments, it will be understood by those of ordinary skill in the art that：Its according to
Can so modify to the technical solution described in foregoing embodiments, either to which part or all technical characteristic into
Row equivalent substitution；And these modifications or replacement, the essence of appropriate technical solution is departed from various embodiments of the present invention technology
The scope of scheme.
Claims (10)
1. the preparation method for the electric heating film that a kind of graphene oxide is modified, it is characterised in that the electric heating film includes stacked
Conductive layer and heating layer；
The heating layer is the layer that the ink containing graphene oxide is formed by irradiation；
The ink containing graphene oxide includes at least graphene oxide, water, free radical scavenger and resinoid bond.
2. preparation method according to claim 1, it is characterised in that the dosage rate of the irradiation is 1-600KGy/h, excellent
Choosing using cobalt -60 (60Co) gamma-ray radiation source or electron accelerator carry out the irradiation.
3. preparation method according to claim 1, it is characterised in that in the ink containing graphene oxide, aoxidize stone
The concentration of black alkene is 1%-15%, preferably 5%-10%；
Preferably, in the ink of the graphene oxide, the weight ratio of water and free radical scavenger is 1-10:1；
Preferably, in the ink containing graphene oxide, the weight ratio of graphene oxide and resinoid bond is 1:3-12.
4. according to claim 1-3 any one of them preparation methods, it is characterised in that the free radical scavenger is alcohol, amine
With the one or more in ketone；The alcohol is preferably selected from the one or more in methanol, ethanol and isopropanol；The amine preferably selects
One or more from monoethanolamine, diethanol amine and triethanolamine, preferably triethanolamine；The ketone is preferably acetone or butanone
Or both mixing.
5. preparation method according to claim 1, it is characterised in that the resinoid bond is epoxy resin, acrylic acid
One or more in resin and organic siliconresin, preferred epoxy.
6. preparation method according to claim 1 or 5, it is characterised in that the ink is also comprising photoinitiator, crosslinking agent
At least one of with diluent.
7. preparation method according to claim 6, it is characterised in that the photoinitiator includes diazol, Diaryl iodonium
One or more mixing in salt, triaryl sulfonium salts, alkyl sulfosalt, iron arene salt, sulfonyloxy ketone and triaryl silica ether, it is excellent
Select diaryl group iodized salt；
Preferably, the crosslinking agent is in alkenes crosslinking agent, organic silicon crosslinking agent and epichlorohydrin resin class crosslinking agent
It is one or more of；The alkenes crosslinking agent is preferably selected from polyethyleneglycol diacrylate, polyethylene polyamine, three allyl of melamine
One or more in ester, triallyl cyanurate, trimethylolpropane tris-(3- aziridinyls)-propionic ester；It is described to have
Machine silicon class crosslinking agent is preferably silane coupling agent；The epichlorohydrin resin class crosslinking agent is preferably crosslinking agent DE；
Preferably, the diluent is TMPTA, TPGDA, HDDA, DPGDA, EO-TMPTA, lauryl diglycidyl ether, second
One or more in glycol glycidol ether, trimethylolpropane glycidol ether and toluene glycidol ether.
8. preparation method according to claim 1, it is characterised in that the conductive layer includes silver electrode layer and copper electrode
Layer；
Preferably, the thickness of the heating layer is 8-30 μm, preferably 10-15 μm；
Preferably, the outer surface of the electric heating film is provided with insulating layer.
9. the electric heating film that a kind of graphene oxide is modified, it is characterised in that prepared using claim 1-8 any one of them
Method is made.
10. the application for the electric heating film that the graphene oxide described in claim 9 is modified, it is characterised in that the electric heating film
For heating equipment.
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| CN109673066A (en) * | 2018-12-06 | 2019-04-23 | 天津中亚慧通科技有限公司 | A kind of preparation method of automobile rearview mirror electric heating film |
| CN111116056A (en) * | 2019-12-31 | 2020-05-08 | 华南理工大学 | Super-hydrophobic thin film with electrochromic effect by electric heating and preparation method thereof |
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