CN108696953A - A kind of high temperature resistant, solvent resistant silicon rubber base Flexible graphene heating film - Google Patents
A kind of high temperature resistant, solvent resistant silicon rubber base Flexible graphene heating film Download PDFInfo
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- CN108696953A CN108696953A CN201710236217.6A CN201710236217A CN108696953A CN 108696953 A CN108696953 A CN 108696953A CN 201710236217 A CN201710236217 A CN 201710236217A CN 108696953 A CN108696953 A CN 108696953A
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- graphene
- silicones
- silicon rubber
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Classifications
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- 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—Heater elements characterised by the composition or nature of the materials or by the arrangement of the conductor
- H05B3/12—Heater 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—Heater 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
-
- 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
- H05B3/34—Heating elements having extended surface area substantially in a two-dimensional plane, e.g. plate-heater flexible, e.g. heating nets or webs
- H05B3/36—Heating elements having extended surface area substantially in a two-dimensional plane, e.g. plate-heater flexible, e.g. heating nets or webs heating conductor embedded in insulating material
Abstract
The present invention relates to a kind of high temperature resistants, the preparation method of solvent resistant silicon rubber base Flexible graphene heating film, solvent resistance silicon rubber is added with the graphene and heat resistance additive of silicones cladding processing, it stirs simultaneously, obtain evenly dispersed silicon rubber base graphene dispersing solution, crosslinking agent and catalyst are added in dispersion liquid, removing bubble is vacuumized after mixing, then it is coated on release film, certain thickness coating layer is formed after drying, then vulcanize 0.5~3h at 50~200 DEG C, graphene flexible high-temperature resistant solvent-resisting composite silicone rubber membrane is obtained after being cooled to room temperature.The present invention is using solvent-resisting silicon rubber flexible as matrix, using the graphene of silicones cladding processing and heat resistance additive as filler, graphene, heat resistance additive are dispersed in silicone rubber matrix, not only conductive but also fever and high temperature resistant, solvent resistant, under lower applied voltage, it is achieved with very high surface temperature, is formed under lower content conductive, is conducive to that processing machinery performance is good and the conductive and heating composite film of flexible deformable.
Description
Technical field
The present invention relates to the preparation methods of flexible high-temperature resistant, solvent resistance polymer matrix conductive and heating film, more specifically,
More particularly to a kind of high temperature resistant, the preparation method of solvent resistant silicon rubber base Flexible graphene heating film..
Background technology
The mode and material for being presently available for heating have very much, including electrical heating, infrared heating and electromagnetic heating etc..By
High, easy to use in the efficiency of heating surface, electrical heating is widely used general.It is mainly electric conductor for electrically heated material, wherein leading
Electric body includes metallic conductor and polymer conductivity.Due to preparing, simple, density is low and flexibility is good, polymer-matrix electric conduction
Composite material, which is widely used in, makes conductive exothermal material.The development of society is more and more high to conductive exothermal material requirements, such as wants
Heater is asked to have preferable flexible, energy random variation is resistant to high temperature, is resistant to solvent etc., is suitable for different fields
The use of conjunction, therefore changeability flexible and high temperature resistant solvent-resisting conductive heating unit gradually draw attention.
It is existing:101928422 A of CN disclose a kind of preparation method of polymer matrix conductive and heating composite film material, gather
Object matrix is closed using polyethylene or the mixture of polyethylene and ethylenic copolymer, conductive exothermal filler uses carbon fiber or nickel plating
Carbon fiber, solution or mixing melting method composite, compacting film forming obtain conductive exothermal composite membrane of polymer;Then by conductive exothermal
Composite membrane of polymer room temperature gamma ray radiation crosslinking Treatment reheats processing removal free radical, obtains final sample.This is compound
Material has preferable heating efficiency, but preparation process is complicated and matrix uses polyethylene, flexible low, non-refractory and solvent.
104159348 A of CN disclose a kind of high heating power Electric radiant Heating Film production method of flexible large area, and electric-heating thin film includes conductive thin
Film, the both ends of conductive film connect copper electrode, and conductive film and the copper electrode that is attached thereto are by the film-insulated sealing of ambroin.
Though the product made has certain flexibility, under certain deformation, conductive network destructible, and same non-refractory and molten
Agent.
Therefore it is current urgently to be resolved hurrily to develop one kind having satisfactory electrical conductivity and high temperature resistant, solvent resistant flexibility heating conductor
The problem of.
Invention content
The purpose of the present invention is be directed to above-mentioned present situation, it is desirable to provide a kind of heating temperature is high, is 50% hair in elongation strain
Hot temperature retentivity is good, high mechanical strength, flexible deformable, solvent resistant, high temperature resistant graphene heating film preparation method.
The object of the invention is achieved in that, a kind of high temperature resistant, solvent resistant silicon rubber base Flexible graphene are generated heat film preparation
Method, preparation are as follows:
1) 100 parts of graphene powders are weighed, with being filtered after silicones/carbitol acetate ester solution impregnation, at room temperature
It is dried to obtain the graphene powder of silicones cladding processing;
Single-layer or multi-layer graphene of the Graphene powder tablet diameter at 0.001 μm~10 μm;
The silicones is methyl phenyl silicone resin, vinyl polysiloxane, methyl hydrogen silicones etc..
2) 100 parts of silicon rubber, 10~100 parts of heat resistance additives are weighed, at 10~100 parts of step 1) silicones claddings
The graphene powder of reason, 0.5~1h of stirring at low speed under normal temperature and pressure in kneader, middle height under then being depressurized at 100~150 DEG C
Speed 2~3h of stirring, 2~3 acquisition base-materials are ground on three-roll grinder, 10~300 parts of volatile organic solvents are then added,
Liquid silastic base graphene dispersing solution is obtained after stirring evenly;
The silicon rubber is single envelope vinyl polysiloxane containing methyl trifluoro propyl or double envelopes containing methyl trifluoro propyl
Vinyl polysiloxane;
The heat resistance additive is FeOOH, di-iron trioxide or acetylene carbon black, and single use or collocation use, preferred
The processed specific surface area of organic titanate is in 10m2The acetylene carbon black of/g or more, use level is at 5~30 parts;
The volatile organic solvent is toluene, dimethylbenzene, ethyl acetate, petroleum ether, positive flow silane, n-pentadecane, hexadecane
And ring hexadecane etc..
3) 0 .05~2 part catalyst and 1~10 part is added in the liquid silastic base graphene dispersing solution of step 2)
Crosslinking agent, 3~5h of mixing obtains silicon rubber base graphene dispersing solution in planetary stirrer, and dispersion liquid is filtered and is vacuumized and is removed
Bubble is removed, is then coated on release film, certain thickness coating layer is formed after dry, then vulcanizes 0.5 at 50~200 DEG C
~3h obtains the flexible high-temperature resistant solvent-resisting composite silicone rubber membrane for mixing graphene after being cooled to room temperature;
The crosslinking agent be reactive hydrogen block methylhydrogenpolysi,oxane, methyl blocking methylhydrogenpolysi,oxane, phenyl hydrogen-containing silicon oil,
Methyl hydrogen MQ silicones, the MQ silicones of hydrogen containing phenyl methyl etc.;
The catalyst is platinum-vinyl siloxane composition catalyst, chloroplatinic acid catalyst, alcohol are modified chloroplatinic acid catalyst,
Platinum-alkynes basigamy mixture catalyst etc..
Advantages of the present invention:
1, it is provided using addition-type silicon rubber containing methyl trifluoro propyl flexible so that heater has flexible, deformability and resistance to
Solvent;
2, processing graphene is simply coated using silicones, improves the compatibility of graphene and silicone rubber matrix so that stone
Black alkene can be dispersed in silicone rubber matrix, and conduction can be formed under low filling, be conducive to the flexibility for keeping silicon rubber
And changeability;In addition, the mechanical performance of composite membrane is also improved;
3, heat resistance additive is utilized so that composite membrane can be in 300 DEG C or more applied at elevated temperature.
Specific implementation mode
The present invention will weigh graphene powder, with being filtered after silicones/carbitol acetate ester solution impregnation, in room temperature
Under be dried to obtain silicones cladding processing graphene powder;The silicones be methyl phenyl silicone resin, vinyl polysiloxane,
Methyl hydrogen silicones.Weigh the graphene powder that appropriate silicon rubber, heat resistance additive, above-mentioned silicones cladding are handled, stirring
It uniformly obtains base-material and suitable volatile organic solvent is then added into base-material, liquid silastic base is obtained after stirring evenly
Graphene dispersing solution;The silicon rubber is that the list containing methyl trifluoro propyl seals vinyl polysiloxane or contains methyl trifluoro third
Double envelope vinyl polysiloxane of base;The heat resistance additive be FeOOH, di-iron trioxide or acetylene carbon black,
Single use or collocation use, and the preferably processed specific surface area of organic titanate is in 10m2The acetylene carbon black of/g or more;It is described
Volatile organic solvent is toluene, dimethylbenzene, ethyl acetate, petroleum ether, positive flow silane, n-pentadecane, hexadecane and ring 16
Alkane etc., preferably long chain alkane.Suitable catalyst and crosslinking agent is added in aforesaid liquid silicon rubber base graphene dispersing solution, mixes
It closes uniform filtering and vacuumizes removing bubble, be then coated on release film, form certain thickness coating layer after dry, then
Vulcanize 0.5~3h at 50~200 DEG C, obtains the flexible high-temperature resistant solvent-resisting composite silicone rubber membrane for mixing graphene;It is described
Crosslinking agent is that reactive hydrogen blocks methylhydrogenpolysi,oxane, methyl blocking methylhydrogenpolysi,oxane, phenyl hydrogen-containing silicon oil, methyl hydrogen MQ
Silicones, the MQ silicones of hydrogen containing phenyl methyl;The catalyst is platinum-vinyl siloxane composition catalyst, chloroplatinic acid is urged
Agent, alcohol are modified chloroplatinic acid catalyst, platinum-alkynes basigamy mixture catalyst.
The present invention is described in detail with specific embodiment below.
Embodiment 1 weighs 100 parts of piece diameters, 1 μm of multi-layer graphene powder, with silicones/carbitol acetate ester solution impregnation
After filter, be dried at room temperature for obtaining the graphene powder of silicones cladding processing.100 parts of viscosity are added in kneader(25
℃)2000mPas containing the double envelope vinyl polysiloxane of methyl trifluoro propyl, 20 parts of above-mentioned claddings treated graphite
Alkene powder, 10 parts of processed specific surface areas of titanate esters are in 10m2The acetylene carbon black of/g or more, normal temperature and pressure stir 0.5h, then
150 DEG C are warming up to, 2h is stirred under low pressure, slurry is ground 2-3 times on three-roll grinder, is transferred to planetary stirrer, is added 30
Part positive flow silane, 5 parts of methyl hydrogen MQ silicones, 0.5 part of platinum-vinyl siloxane composition catalyst are uniformly mixed under room temperature
To dispersed paste, dispersed paste is filtered to and vacuumized removing bubble, is then coated on release film, thickness is formed after dry
The coating layer of 0.5mm, heating 20min is allowed to complete cure in 120 DEG C of baking ovens, and silicon rubber base Flexible graphene is obtained after cooling
Composite membrane.
Embodiment 2, with embodiment 1, unlike, substitute 1 μm of multi-layer graphene using 5 μm of multi-layer graphene powders of piece diameter
Powder.
Embodiment 3, with embodiment 1, unlike, substitute 1 μm of Multi-layer graphite using 20 μm of multi-layer graphene powders of piece diameter
Alkene powder.
Embodiment 4, with embodiment 1, unlike, add 20 parts of claddings treated that graphene powder replaces with addition 10
Part cladding treated graphene powder.
Embodiment 5, with embodiment 1, unlike, treated that graphene powder replaces with 30 parts of packets of addition for 20 parts of claddings
The graphene powder that covers that treated.
Comparative example 1, with embodiment 1, unlike, be not added with the processed specific surface area of titanate esters in 10m2The second of/g or more
Alkynes carbon black.
Comparative example 2 weighs 100 parts of piece diameters, 1 μm of multi-layer graphene powder, is impregnated with silicones/carbitol acetate ester solution
It is filtered after processing, is dried at room temperature for obtaining the graphene powder of silicones cladding processing.100 parts of viscosity are added in kneader
(25℃)Double envelope vinyl polysiloxane of 2000mPas, 20 parts of above-mentioned claddings treated graphene powder, room temperature
Atmospheric agitation 0.5h then heats to 150 DEG C, and 2h is stirred under low pressure, and slurry grinds 2~3 times on three-roll grinder, is transferred to
30 parts of positive flow silanes, 5 parts of methyl hydrogen MQ silicones, 0.5 part of platinum-vinyl siloxane composition catalyst is added in planetary stirrer,
It is uniformly mixed under room temperature and obtains dispersed paste, dispersed paste is filtered to and vacuumized removing bubble, is then coated on release film,
The coating layer of thickness 0.5mm is formed after drying, heating 20min is allowed to complete cure in 120 DEG C of baking ovens, and silicon rubber is obtained after cooling
Matrix Flexible graphene composite membrane.
100 parts of viscosity are added in comparative example 3 in kneader(25℃)Double envelope vinyl polysiloxane of 2000mPas,
20 parts of untreated graphene powders, 10 parts of processed specific surface areas of titanate esters are in 10m2The acetylene carbon black of/g or more, often
Normal temperature and pressure stirs 0.5h, then heats to 150 DEG C, 2h is stirred under low pressure, and slurry is ground 2-3 times on three-roll grinder, transfer
To planetary stirrer, it is complex-catalyzed that 30 parts of positive flow silanes, 5 parts of methyl hydrogen MQ silicones, 0.5 part of platinum-vinyl siloxane is added
Agent is uniformly mixed under room temperature and obtains dispersed paste, dispersed paste is filtered to and vacuumized removing bubble, is then applied on release film
Cloth forms the coating layer of thickness 0.5mm after dry, heating 20min is allowed to complete cure in 120 DEG C of baking ovens, and silicon is obtained after cooling
Rubber-base flexible graphene composite film.
Each embodiment crumples the surface under experiment and stretching and bending in 10V and 15V voltages underlaying surface temperature and in skot
Temperature see the table below:(sample size is length * width * thickness=10cm*5cm*0.5mm)
Physical mechanical property and the surface temperature under 300 DEG C of degradations of each embodiment see the table below:(sample size is length *
Width * thickness=10cm*5cm*1mm)
The solvent resistance result of each embodiment see the table below:(sample size is length * width * thickness=2cm*2cm*2cm)
From in above-mentioned table as can be seen that graphene by silicones cladding processing after gained flexible silicone rubber base graphene heating film
High in the lower heating temperature of loading, temperature does not have reduction apparent in the case of rubbing repeatedly, in high temperature ageing and answers
In the case of becoming larger, heating temperature retentivity is good and has good solvent resistance.
Claims (4)
1. the preparation method of a kind of high temperature resistant, solvent resistant silicon rubber base Flexible graphene heating film, it is characterised in that:Specific steps
It is as follows:
1) 100 parts of graphene powders are weighed, with being filtered after silicones/carbitol acetate ester solution impregnation, are done at room temperature
It is dry to obtain the graphene powder of silicones cladding processing;
The graphene powder is single-layer or multi-layer graphene of the piece diameter at 0.001 μm~10 μm;
Silicones is methyl phenyl silicone resin, vinyl polysiloxane, methyl hydrogen silicones etc.;
2) 100 parts of silicon rubber, 10~100 parts of heat resistance additives, 10~100 parts of step 1) silicones claddings are weighed to handle
Graphene powder stirs evenly acquisition base-material, then, 10~300 parts of volatile organic solvents is added into base-material, stir evenly
Liquid silastic base graphene dispersing solution is obtained afterwards;
The silicon rubber is single envelope vinyl polysiloxane containing methyl trifluoro propyl or double envelopes containing methyl trifluoro propyl
Vinyl polysiloxane;
The heat resistance additive is FeOOH, di-iron trioxide or acetylene carbon black, and single use or collocation use, preferred
The processed specific surface area of organic titanate is in 10m2The acetylene carbon black of/g or more, use level is at 5-30 parts;
The volatile organic solvent is toluene, dimethylbenzene, ethyl acetate, petroleum ether, positive flow silane, n-pentadecane, hexadecane
And ring hexadecane etc..
2.3) 0 .05 parts~2 parts catalyst and 1~10 part are added in the liquid silastic base graphene dispersing solution of step 2)
Crosslinking agent is uniformly mixed and obtains silicon rubber base graphene dispersing solution, filters, vacuumizes removing bubble, then applied on release film
Cloth forms certain thickness coating layer after dry, then vulcanizes 0.5~3h at 50~200 DEG C, is mixed after being cooled to room temperature
The flexible high-temperature resistant solvent-resisting composite silicone rubber membrane of miscellaneous graphene;
The crosslinking agent be reactive hydrogen block methylhydrogenpolysi,oxane, methyl blocking methylhydrogenpolysi,oxane, phenyl hydrogen-containing silicon oil,
Methyl hydrogen MQ silicones, the MQ silicones of hydrogen containing phenyl methyl etc.;
The catalyst is platinum-vinyl siloxane composition catalyst, chloroplatinic acid catalyst, alcohol are modified chloroplatinic acid catalyst,
Platinum-alkynes basigamy mixture catalyst etc..
3. the preparation method of a kind of high temperature resistant according to claim 1, solvent resistant silicon rubber base Flexible graphene heating film,
It is characterized in that:The Graphene powder tablet diameter described in step 1) is in 0.001 μm~10 μm single-layer or multi-layer graphenes;
Cladding is methyl phenyl silicone resin, vinyl polysiloxane, methyl hydrogen silicones etc. with silicones;Silicon rubber described in step 2)
Glue is vinylsiloxane rubber containing methyl trifluoro propyl;Heat resistance additive described in step 2) is FeOOH, three oxidations two
Iron or acetylene carbon black, single use or collocation use, and the preferred processed specific surface area of organic titanate is in 10m2/ g's or more
Acetylene carbon black;Step 2) the volatile organic solvent is toluene, dimethylbenzene, ethyl acetate, petroleum ether, positive flow silane, positive 15
Alkane, hexadecane and ring hexadecane etc..
4. the fever of a kind of high temperature resistant according to claim 1, solvent resistance silicon rubber base flexible deformable graphene is compound
The preparation method of film, it is characterised in that:The agitating mode of base-material is 0.5~1h of stirring at low speed under normal temperature and pressure in step 2), so
High speed stirs 2~3h under being depressurized afterwards at 100~150 DEG C, is ground 2~3 times on three-roll grinder, being cooled to room temperature addition has
Solvent normal temperature and pressure mixes.
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| CN201710236217.6A CN108696953A (en) | 2017-04-12 | 2017-04-12 | A kind of high temperature resistant, solvent resistant silicon rubber base Flexible graphene heating film |
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| CN201710236217.6A CN108696953A (en) | 2017-04-12 | 2017-04-12 | A kind of high temperature resistant, solvent resistant silicon rubber base Flexible graphene heating film |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108299830A (en) * | 2018-02-07 | 2018-07-20 | 杭州白熊科技有限公司 | Silicon rubber base Flexible graphene heating film and preparation method thereof, heating device and application |
| CN109629706A (en) * | 2018-11-29 | 2019-04-16 | 牛墨石墨烯应用科技有限公司 | A kind of assembled graphene fever wallboard |
| CN110149738A (en) * | 2019-04-22 | 2019-08-20 | 杭州电子科技大学 | It is a kind of based on graphene/ferric oxide composite material Electric radiant Heating Film and preparation method thereof |
| CN112920704A (en) * | 2019-12-05 | 2021-06-08 | 中车唐山机车车辆有限公司 | Electric heating coating paint, electric heating skin and ice and snow prevention system |
-
2017
- 2017-04-12 CN CN201710236217.6A patent/CN108696953A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108299830A (en) * | 2018-02-07 | 2018-07-20 | 杭州白熊科技有限公司 | Silicon rubber base Flexible graphene heating film and preparation method thereof, heating device and application |
| CN108299830B (en) * | 2018-02-07 | 2021-02-23 | 杭州白熊科技有限公司 | Silicone rubber-based flexible graphene heating film, preparation method thereof, heating device and application |
| CN109629706A (en) * | 2018-11-29 | 2019-04-16 | 牛墨石墨烯应用科技有限公司 | A kind of assembled graphene fever wallboard |
| CN110149738A (en) * | 2019-04-22 | 2019-08-20 | 杭州电子科技大学 | It is a kind of based on graphene/ferric oxide composite material Electric radiant Heating Film and preparation method thereof |
| CN112920704A (en) * | 2019-12-05 | 2021-06-08 | 中车唐山机车车辆有限公司 | Electric heating coating paint, electric heating skin and ice and snow prevention system |
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