CN110126368A - A kind of electric heating rubber and preparation method thereof - Google Patents
A kind of electric heating rubber and preparation method thereof Download PDFInfo
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- CN110126368A CN110126368A CN201910368023.0A CN201910368023A CN110126368A CN 110126368 A CN110126368 A CN 110126368A CN 201910368023 A CN201910368023 A CN 201910368023A CN 110126368 A CN110126368 A CN 110126368A
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- 238000005485 electric heating Methods 0.000 title claims abstract description 118
- 229920001971 elastomer Polymers 0.000 title claims abstract description 92
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000000463 material Substances 0.000 claims abstract description 69
- 238000010438 heat treatment Methods 0.000 claims abstract description 58
- 229910052751 metal Inorganic materials 0.000 claims abstract description 17
- 239000002184 metal Substances 0.000 claims abstract description 17
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- 238000001035 drying Methods 0.000 claims description 26
- 239000003795 chemical substances by application Substances 0.000 claims description 23
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 21
- 238000001816 cooling Methods 0.000 claims description 20
- 239000007822 coupling agent Substances 0.000 claims description 20
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 20
- 238000005096 rolling process Methods 0.000 claims description 20
- 239000002002 slurry Substances 0.000 claims description 19
- 229920002943 EPDM rubber Polymers 0.000 claims description 18
- 238000004073 vulcanization Methods 0.000 claims description 16
- 238000005303 weighing Methods 0.000 claims description 16
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical group CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 15
- 239000011248 coating agent Substances 0.000 claims description 14
- 238000000576 coating method Methods 0.000 claims description 14
- 239000011231 conductive filler Substances 0.000 claims description 14
- 239000011810 insulating material Substances 0.000 claims description 13
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 12
- 239000003085 diluting agent Substances 0.000 claims description 12
- 238000010304 firing Methods 0.000 claims description 10
- 238000007731 hot pressing Methods 0.000 claims description 10
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 239000000853 adhesive Substances 0.000 claims description 8
- 230000001070 adhesive effect Effects 0.000 claims description 8
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 claims description 8
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 8
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 8
- 239000002904 solvent Substances 0.000 claims description 8
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 7
- 235000013527 bean curd Nutrition 0.000 claims description 7
- 239000000945 filler Substances 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 6
- 239000004642 Polyimide Substances 0.000 claims description 6
- 239000004917 carbon fiber Substances 0.000 claims description 6
- 239000003822 epoxy resin Substances 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 6
- 239000004014 plasticizer Substances 0.000 claims description 6
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 claims description 6
- 229920000647 polyepoxide Polymers 0.000 claims description 6
- 229920001721 polyimide Polymers 0.000 claims description 6
- 239000002952 polymeric resin Substances 0.000 claims description 6
- 229920005989 resin Polymers 0.000 claims description 6
- 239000011347 resin Substances 0.000 claims description 6
- 229920003002 synthetic resin Polymers 0.000 claims description 6
- 239000011521 glass Substances 0.000 claims description 5
- 239000003365 glass fiber Substances 0.000 claims description 5
- 239000004005 microsphere Substances 0.000 claims description 5
- 239000003973 paint Substances 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 229910021389 graphene Inorganic materials 0.000 claims description 4
- 229910002804 graphite Inorganic materials 0.000 claims description 4
- 239000010439 graphite Substances 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 239000012774 insulation material Substances 0.000 claims description 2
- 239000004020 conductor Substances 0.000 claims 1
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- 238000005470 impregnation Methods 0.000 description 6
- 238000010907 mechanical stirring Methods 0.000 description 5
- 239000011325 microbead Substances 0.000 description 5
- 229920002379 silicone rubber Polymers 0.000 description 5
- 238000006359 acetalization reaction Methods 0.000 description 3
- 238000010790 dilution Methods 0.000 description 3
- 239000012895 dilution Substances 0.000 description 3
- 230000005855 radiation Effects 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 230000032683 aging Effects 0.000 description 2
- 238000005452 bending Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910000623 nickel–chromium alloy Inorganic materials 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 230000005653 Brownian motion process Effects 0.000 description 1
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- 238000005537 brownian motion Methods 0.000 description 1
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- 150000001723 carbon free-radicals Chemical class 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
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- 238000009776 industrial production Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- PVFSDGKDKFSOTB-UHFFFAOYSA-K iron(3+);triacetate Chemical compound [Fe+3].CC([O-])=O.CC([O-])=O.CC([O-])=O PVFSDGKDKFSOTB-UHFFFAOYSA-K 0.000 description 1
- 244000144972 livestock Species 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
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- 230000002285 radioactive effect Effects 0.000 description 1
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- 238000003860 storage Methods 0.000 description 1
- 239000000052 vinegar Substances 0.000 description 1
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B17/00—Layered products essentially comprising sheet glass, or glass, slag, or like fibres
- B32B17/06—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B25/00—Layered products comprising a layer of natural or synthetic rubber
- B32B25/04—Layered products comprising a layer of natural or synthetic rubber comprising rubber as the main or only constituent of a layer, which is next to another layer of the same or of a different material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B3/00—Layered products comprising a layer with external or internal discontinuities or unevennesses, or a layer of non-planar shape; Layered products comprising a layer having particular features of form
- B32B3/10—Layered products comprising a layer with external or internal discontinuities or unevennesses, or a layer of non-planar shape; Layered products comprising a layer having particular features of form characterised by a discontinuous layer, i.e. formed of separate pieces of material
- B32B3/12—Layered products comprising a layer with external or internal discontinuities or unevennesses, or a layer of non-planar shape; Layered products comprising a layer having particular features of form characterised by a discontinuous layer, i.e. formed of separate pieces of material characterised by a layer of regularly- arranged cells, e.g. a honeycomb structure
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B33/00—Layered products characterised by particular properties or particular surface features, e.g. particular surface coatings; Layered products designed for particular purposes not covered by another single class
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
- B32B5/16—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by features of a layer formed of particles, e.g. chips, powder or granules
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2260/00—Layered product comprising an impregnated, embedded, or bonded layer wherein the layer comprises an impregnation, embedding, or binder material
- B32B2260/02—Composition of the impregnated, bonded or embedded layer
- B32B2260/021—Fibrous or filamentary layer
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2260/00—Layered product comprising an impregnated, embedded, or bonded layer wherein the layer comprises an impregnation, embedding, or binder material
- B32B2260/04—Impregnation, embedding, or binder material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2262/00—Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
- B32B2262/10—Inorganic fibres
- B32B2262/101—Glass fibres
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2264/00—Composition or properties of particles which form a particulate layer or are present as additives
- B32B2264/10—Inorganic particles
- B32B2264/101—Glass
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2307/00—Properties of the layers or laminate
- B32B2307/20—Properties of the layers or laminate having particular electrical or magnetic properties, e.g. piezoelectric
- B32B2307/202—Conductive
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2307/00—Properties of the layers or laminate
- B32B2307/30—Properties of the layers or laminate having particular thermal properties
- B32B2307/302—Conductive
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Wood Science & Technology (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Resistance Heating (AREA)
Abstract
The invention discloses a kind of electric heating rubber, including thermal insulation layer, conductive heating layer and insulated thermal insulating layer, and conductive heating layer is between thermal insulation layer and insulated thermal insulating layer；Wherein, conductive heating layer is the flexible electric heating material with conductive heater function, and the metal current-carrying item as electrode is provided on conductive heating layer.The invention also discloses a kind of preparation methods of electric heating rubber.Electric heating rubber of the invention has the advantages that fever is uniform, heating rate is fast, electric conversion efficiency is high, application field is wide, production cost is low.
Description
Technical Field
The invention relates to the field of materials, in particular to an electric heating rubber and a preparation method thereof.
Background
The electric heating rubber is, as the name implies, rubber that can be heated after being energized. The electric heating rubber has wide application in production and life, and can be realized by adopting the electric heating rubber as a heat insulation sleeve required in industrial production and a heating pad in a cold environment.
The electric heating rubber in the prior art has various implementation modes, for example, in the Chinese utility model patent with the publication number of "CN 208479974U" and the name of "a silicon rubber electric heating belt", a structure of the silicon rubber electric heating belt is disclosed. The silicon rubber electric heating tape wraps silicon rubber on the nickel-chromium alloy electric heating wire, and the nickel-chromium alloy electric heating wire generates heat after being electrified so as to heat the external silicon rubber. The electric heating rubber similar to the structure is very common, and the structure has various changes, such as using electric heating wires with other component types or winding and bending the electric heating wires to enlarge the heating area. The electric heating rubber has the problem of uneven heating due to the limited area of the electric heating wire, and the problem cannot be fundamentally solved even if the electric heating wire is wound and bent to enlarge the heating area. In addition, although the heating wire may be bent to some extent, if the number of bending times is too large, the heating wire may be broken, which may affect the heating effect of the electric heating rubber. In the prior art, there is an example of replacing the heating wire in the electric heating rubber with the electric heating sheet, which can solve the problem of uneven heating to a certain extent, but the electric heating sheet is generally in a hard structure form mainly composed of metal components, so that the problem that the electric heating rubber on which the electric heating sheet is mounted cannot be freely bent is more serious, the matching degree between the electric heating rubber and the shape of the object to be served is influenced, and further the full play of the heat conduction efficiency of the electric heating rubber is influenced. In addition, the thickness of the whole electric heating rubber is increased by the electric heating piece, so that the electric heating rubber cannot be applied to certain scenes with specific requirements on the thickness.
In the chinese utility model patent with the publication number "CN 2502479Y" and the name "rubber electrothermal structure", an electrothermal rubber sheet formed by mixing carbon black, metal powder and rubber is disclosed, one side of the electrothermal rubber sheet is provided with a main conductive sheet with low resistance, the other side is provided with an auxiliary conductive sheet with low resistance, and the main conductive sheet and the auxiliary conductive sheet are respectively connected with the positive and negative electrodes to form an electronic loop. The applicant believes that the electric heating rubber sheet is soft in texture and can be bent and folded at will, and the problem that the electric heating rubber provided with the electric heating sheet cannot be bent freely is solved. After research, the applicant believes that the electric heating rubber sheet has the problems of not high heating speed, not high electric heating radiation conversion efficiency and the like due to the fact that various materials such as carbon black, rubber and the like are mixed.
Disclosure of Invention
The invention aims to overcome the defects of nonuniform heating, low heating temperature, low heating speed and the like of the electric heating rubber in the prior art, thereby providing the electric heating rubber with uniform heating, high heating speed, high electric heating conversion efficiency, wide application field and low production cost.
In order to achieve the above purpose, the present invention provides an electric heating rubber, which comprises an insulating heat conduction layer 1, an electric conduction heating layer 2 and an insulating heat insulation layer 3, wherein the electric conduction heating layer 2 is located between the insulating heat conduction layer 1 and the insulating heat insulation layer 3; wherein,
the conductive heating layer 2 is a flexible electric heating material with a conductive heating function, and a metal current carrying strip 5 serving as an electrode is arranged on the conductive heating layer 2.
In the technical scheme, the insulating and heat-insulating layer 3 adopts hollow microspheres with the diameter of 10-100 mu m as heat-insulating filler.
In the technical scheme, the conductive heating layer 2 is in a grid shape, and the mesh number range is 4-20 meshes, so that a uniform conductive network is formed.
The invention also provides a preparation method of the electric heating rubber, which comprises the following steps:
immersing the prepreg cloth in the conductive coating, stirring and immersing, taking out the prepreg cloth with the conductive coating, flattening, and drying to obtain an electric heating material;
preparing an insulating material;
preparing an insulating heat conduction material;
stacking the insulating heat conduction material, the electric heating material, the metal current carrying strip and the insulating heat insulation material in sequence, and then carrying out firing hot pressing in a vulcanizing machine to obtain the electric heating rubber to be prepared; wherein the vulcanization temperature is between 100 and 300 ℃, and the vulcanization pressure is between 5 and 20 MPa.
In the above technical scheme, the conductive coating is a water-based conductive coating, and the preparation of the water-based conductive coating comprises the following steps:
weighing 30-60% of waterborne polymer resin, adding 3-8% of coupling agent diluted by diluent, adding 5-40% of modified conductive filler into the waterborne polymer resin added with the coupling agent, and then grinding for 20-60 min to uniformly disperse the modified conductive filler to obtain waterborne conductive slurry; wherein,
the waterborne polymer resin adopts one or two of epoxy resin and polyimide; the diluent adopts one or two of acetone, MD212 and deionized water; the coupling agent is one or two of a ferrate coupling agent and a coupling agent KH 550; the conductive filler is one or two of graphite, carbon black, graphene and chopped carbon fiber.
In the above technical scheme, the conductive coating is an oily conductive coating, and the oily conductive coating is obtained by preparation, and the preparation of the oily conductive coating comprises the following steps:
weighing 10-30% of adhesive by mass, 60-90% of solvent by mass, dissolving the adhesive in the solvent, then weighing 2-10% of modified conductive filler, adding the conductive filler into the solvent in which the adhesive is dissolved, and finally grinding for 20-60 min to uniformly disperse the conductive filler to obtain oily conductive slurry; wherein,
the adhesive is polyvinyl butyral resin, the solvent is dimethylformamide, and the conductive filler is one or two of graphite, carbon black, graphene and chopped carbon fiber.
In the technical scheme, the pre-impregnated cloth is made of one of bean curd cloth and glass fiber mesh cloth, and the mesh number of the pre-impregnated cloth ranges from 4 meshes to 20 meshes.
In the above technical scheme, the preparing of the insulating material comprises:
weighing 40-80% of ethylene propylene diene monomer, 5-10% of methyl silicone oil, 2-8% of vulcanizing agent, 3-6% of white carbon black, 3-5% of plasticizer and 5-15% of hollow microspheres according to the mass ratio, mixing in a mixer, banburying, rolling, cooling, warehousing and curing.
In the above technical scheme, the hollow beads are hollow glass beads or hollow alumina beads.
Among the above-mentioned technical scheme, preparation insulating heat conduction material includes:
weighing 30-75% of ethylene propylene diene monomer, 5-10% of methyl silicone oil, 2-8% of vulcanizing agent, 3-6% of white carbon black, 3-5% of plasticizer and 10-25% of high-thermal-conductivity filler according to the mass ratio, and mixing in a mixer; then banburying, rolling, cooling, warehousing and curing are carried out; wherein,
the high-thermal-conductivity filler is one or two of aluminum nitride and silicon carbide.
The invention has the advantages that:
1. the electric heating rubber adopts the net-shaped flexible electric heating material as the electric conduction heating layer, and the electric conduction heating layer forms an even electric conduction network, so that the whole surface heating can be realized, the temperature is uniformly distributed, and hot spots can not be formed for heating; this conductive heating layer embedding has strengthened whole electric heat rubber's intensity on the one hand in insulating rubber, and on the other hand makes it even through buckling the inflection, also can be because of the elasticity of rubber and the reconversion, has solved traditional electric heat rubber heating uneven and the problem that can't buckle many times.
2. The electric heating rubber can realize high-efficiency electric heating conversion, and is more energy-saving and power-saving compared with the traditional electric heating mode.
3. The electric heating rubber is matt and noiseless, is the safest heating body known at present, can greatly expand the application field of the electric heating rubber, and has wide application scenes.
4. The electric heating rubber has high heating speed.
5. The electric heating rubber has high reliability.
6. The electric heating rubber has the advantages of simple processing and low cost.
Drawings
FIG. 1 is a schematic view of an electrothermal rubber of the present invention;
FIG. 2 is a schematic diagram of the division of the electric heating rubber of the present invention;
FIG. 3 is a schematic view of the paving of the electric heating rubber of the present invention;
FIG. 4 is a graph showing the temperature of the electric heating rubber of the present invention as a function of energization time;
FIG. 5 is a graph showing the resistance value of the electric heating rubber of the present invention as a function of the energization time when the surface temperature is room temperature.
Description of the drawings
1 insulating heat-conducting layer 2 conductive heating layer
3 insulating layer 4 electrothermal material
5 Metal Current Carrier strip
Detailed Description
The invention will now be further described with reference to the accompanying drawings.
Example 1
Preparing an aqueous conductive paste comprising: weighing 1 part of the iron acid-vinegar coupling agent by mass, and then mixing the components in a mass ratio of 1: 2, adding acetone for dilution to obtain a diluted coupling agent; 60 parts of epoxy resin is weighed according to the mass, the diluted coupling agent is added into the epoxy resin, 37 parts of modified graphene is added according to the mass, and grinding is carried out for half an hour to ensure that the modified graphene is uniformly dispersed, so that the waterborne conductive paste is obtained.
Preparing an electric heating material, comprising: bean curd cloth with the mesh number of 8 is selected as presoaked cloth to be immersed in the prepared conductive slurry, and mechanical stirring is carried out for 20min during immersion to ensure the uniformity of the immersion of the conductive slurry; taking out and flattening the prepreg cloth soaked with the conductive paste, and drying the prepreg cloth by an infrared dryer to obtain a material with electrothermal property; wherein, the content of the diluent after drying is ensured to be less than 1 percent during drying.
Preparing an insulating and heat-insulating layer material, comprising: methyl silicone oil, a vulcanizing agent, white carbon black, plasticization and hollow glass beads (the diameter is 10 mu m) are mixed according to the proportion of 5: 2: 3: 3: 5, putting the mixture into a mixer for mixing; then banburying, rolling, cooling, warehousing and curing for 12 hours for later use.
Preparing an insulating heat-conducting layer material, comprising: mixing ethylene propylene diene monomer, methyl silicone oil, a vulcanizing agent, white carbon black, plasticizing and aluminum nitride according to the weight ratio of 75: 5: 2: 3: 3: 12, putting the mixture into a mixer for mixing; then banburying, rolling, cooling, warehousing and curing for 12 hours for later use.
And stacking the insulating heat-conducting layer material, the electric heating material, the metal current-carrying strip and the insulating heat-insulating material in sequence, and then carrying out firing hot pressing in a vulcanizing machine to obtain the electric heating rubber composite material to be prepared. Wherein the temperature in the vulcanizing machine during vulcanization is 172 ℃, and the vulcanization pressure is 6 MPa.
Example 2
Preparing an aqueous conductive paste comprising: weighing KH 5504 parts of coupling agent by mass, and then adding MD 2124 parts for dilution to obtain the diluted coupling agent; 60 parts of polyimide is weighed according to the mass, the diluted coupling agent is added into the polyimide, 32 parts of modified graphite is added according to the mass, and the mixture is ground for 20 minutes to be uniformly dispersed, so that the water-based conductive slurry is obtained.
Preparing an electric heating material, comprising: selecting a glass fiber mesh with the mesh number of 4 as a pre-impregnated cloth to be immersed in the prepared conductive paste, and mechanically stirring for 40min during impregnation to ensure the impregnation uniformity of the conductive paste; then taking out and flattening the prepreg cloth soaked with the conductive paste, and drying the prepreg cloth through an infrared dryer to obtain a material with electrothermal property; wherein, the content of the diluent after drying is ensured to be less than 1 percent during drying.
Preparing an insulating and heat-insulating layer material, comprising: mixing ethylene propylene diene monomer, methyl silicone oil, a vulcanizing agent, white carbon black, plasticization and hollow glass beads (the diameter is 100 mu m) according to the proportion of 56: 10: 8: 6: 5: 15, and putting the mixture into a mixer for mixing; then banburying, rolling, cooling, warehousing and curing for 8 hours for later use.
Preparing an insulating heat-conducting layer material, comprising: mixing ethylene propylene diene monomer, methyl silicone oil, a vulcanizing agent, white carbon black, plasticizing agent and silicon carbide according to a proportion of 46: 10: 8: 6: 5: 25, and putting the mixture into a mixer for mixing; then banburying, rolling, cooling, warehousing and curing for 12 hours for later use.
And stacking the insulating heat-conducting layer material, the electric heating material, the metal current-carrying strip and the insulating heat-insulating material in sequence, and then carrying out firing hot pressing in a vulcanizing machine to obtain the electric heating rubber composite material to be prepared. Wherein the temperature in the vulcanizing machine is 100 ℃ and the vulcanizing pressure is 5 MPa.
Example 3
Preparing an aqueous conductive paste comprising: weighing 3 parts of ferric acetate coupling agent and KH550 coupling agent by mass, and adding 3 parts of deionized water by mass for dilution to obtain the diluted coupling agent; weighing 55 parts of epoxy resin and 55 parts of polyimide, adding the diluted coupling agent into the mixture of the epoxy resin and the polyimide, then adding 39 parts of modified chopped carbon fibers by mass, and grinding for half an hour to uniformly disperse the modified chopped carbon fibers, thereby obtaining the aqueous conductive slurry.
Preparing an electric heating material, comprising: bean curd cloth with the mesh number of 20 is selected as presoaked cloth to be immersed in the prepared conductive slurry, and mechanical stirring is carried out for 30min during immersion in order to ensure the uniformity of the immersion of the conductive slurry; then taking out and flattening the prepreg cloth soaked with the conductive paste, and drying the prepreg cloth through an infrared dryer to obtain a material with electrothermal property; wherein, the content of the diluent after drying is ensured to be less than 1 percent during drying.
Preparing an insulating and heat-insulating layer material, comprising: mixing ethylene propylene diene monomer, methyl silicone oil, a vulcanizing agent, white carbon black, plasticization and hollow alumina micro-beads (the diameter is 50 mu m) according to a proportion of 65: 8: 6: 5: 4: 12, putting the mixture into a mixer for mixing; then banburying, rolling, cooling, warehousing and curing for 12 hours for later use.
Preparing an insulating heat-conducting layer material, comprising: mixing ethylene propylene diene monomer, methyl silicone oil, a vulcanizing agent, white carbon black, plasticization, aluminum nitride and silicon carbide according to the weight ratio of 57: 8: 6: 5: 4: weighing 20 parts by mass, and mixing in a mixer; then banburying, rolling, cooling, warehousing and curing for 16 hours for later use.
And stacking the insulating heat-conducting layer material, the electric heating material, the metal current-carrying strip and the insulating heat-insulating material in sequence, and then carrying out firing hot pressing in a vulcanizing machine to obtain the electric heating rubber composite material to be prepared. Wherein the temperature in the vulcanizing machine during vulcanization is 300 ℃, and the vulcanization pressure is 20 MPa.
Example 4
The existing water-based conductive paint is purchased from the market, such as the power heating paint with the model number of 05H06 produced by Shenzhen Seiya electronic paste Limited.
Preparing an electric heating material, comprising: selecting a 16-mesh glass fiber mesh cloth as a pre-impregnated cloth to be immersed in the previously purchased aqueous conductive paste, and mechanically stirring for 25min during impregnation in order to ensure the impregnation uniformity of the conductive paste; taking out and flattening the prepreg cloth soaked with the conductive paste, and drying the prepreg cloth by an infrared dryer to obtain a material with electrothermal property; wherein, the content of the diluent after drying is ensured to be less than 1 percent during drying.
Preparing an insulating and heat-insulating layer material, comprising: methyl silicone oil, a vulcanizing agent, white carbon black, plasticization and hollow alumina micro-beads (the diameter is 60 mu m) are mixed according to the proportion of 8: 6: 5: 4: 9, putting the materials into a mixer for mixing; then banburying, rolling, cooling, warehousing and curing for 12 hours for later use.
Preparing an insulating heat-conducting layer material, comprising: mixing ethylene propylene diene monomer, methyl silicone oil, a vulcanizing agent, white carbon black, plasticizing agent and aluminum nitride according to the weight ratio of 70: 7: 3: 5: 4: 11, putting the mixture into a mixer for mixing; then banburying, rolling, cooling, warehousing and curing for 14 hours for later use.
And stacking the insulating heat-conducting layer material, the electric heating material, the metal current-carrying strip and the insulating heat-insulating material in sequence, and then carrying out firing hot pressing in a vulcanizing machine to obtain the electric heating rubber composite material to be prepared. Wherein the temperature in the vulcanizing machine during vulcanization is 200 ℃, and the vulcanization pressure is 10 MPa.
Example 5
An existing oily conductive coating material such as conductive carbon ink (LN-GCI-1) of Shandong Ritts nanotechnology Co., Ltd is purchased from the market.
Preparing an electric heating material, comprising: bean curd cloth with the mesh number of 12 is selected as presoaked cloth to be immersed in the previously purchased oily conductive slurry, and mechanical stirring is carried out for 35min during immersion in order to ensure the uniformity of the immersion of the conductive slurry; taking out and flattening the prepreg cloth soaked with the conductive paste, and drying the prepreg cloth by an infrared dryer to obtain a material with electrothermal property; wherein, the content of the diluent after drying is ensured to be less than 1 percent during drying.
Preparing an insulating and heat-insulating layer material, comprising: mixing ethylene propylene diene monomer, methyl silicone oil, a vulcanizing agent, white carbon black, plasticizer and hollow alumina micro-beads (the diameter is 30 mu m) according to a proportion of 68: 7: 6: 5: 4: 10, and putting the mixture into a mixer for mixing; then banburying, rolling, cooling, warehousing and curing for 12 hours for later use.
Preparing an insulating heat-conducting layer material, comprising: mixing ethylene propylene diene monomer, methyl silicone oil, a vulcanizing agent, white carbon black, plasticization, aluminum nitride and silicon carbide according to the proportion of 63: 7: 6: 5: 4: 15, and putting the mixture into a mixer for mixing; then banburying, rolling, cooling, warehousing and curing for 9 hours for later use.
And stacking the insulating heat-conducting layer material, the electric heating material, the metal current-carrying strip and the insulating heat-insulating material in sequence, and then carrying out firing hot pressing in a vulcanizing machine to obtain the electric heating rubber composite material to be prepared. Wherein the temperature in the vulcanizing machine during vulcanization is 180 ℃, and the vulcanization pressure is 12 MPa.
Example 6
Preparing oily conductive paste, comprising: 80 parts of polyvinyl butyral resin (molecular weight of 35000) with an acetalization degree of 82 mol% is weighed according to the mass, the polyvinyl butyral resin is dissolved in 400 parts of dimethylformamide weighed according to the mass, then 20 parts of conductive carbon black weighed according to the mass and with the diameter of about 30um is added, and finally, the conductive carbon black is ground for 20 minutes to be uniformly dispersed, so that the oily conductive slurry is obtained.
Preparing an electric heating material, comprising: selecting a glass fiber mesh with the mesh number of 4 as a pre-impregnated cloth to be immersed in the prepared conductive paste, and mechanically stirring for 40min during impregnation to ensure the impregnation uniformity of the conductive paste; then taking out and flattening the prepreg cloth soaked with the conductive paste, and drying the prepreg cloth through an infrared dryer to obtain a material with electrothermal property; wherein, the content of the diluent after drying is ensured to be less than 1 percent during drying.
Preparing an insulating and heat-insulating layer material, comprising: mixing ethylene propylene diene monomer, methyl silicone oil, a vulcanizing agent, white carbon black, plasticization and hollow glass beads (the diameter is 25 mu m) according to the proportion of 56: 10: 8: 6: 5: 15, and putting the mixture into a mixer for mixing; then banburying, rolling, cooling, warehousing and curing for 8 hours for later use.
Preparing an insulating heat-conducting layer material, comprising: mixing ethylene propylene diene monomer, methyl silicone oil, a vulcanizing agent, white carbon black, plasticizing agent and silicon carbide according to a proportion of 46: 10: 8: 6: 5: 25, and putting the mixture into a mixer for mixing; then banburying, rolling, cooling, warehousing and curing for 12 hours for later use.
And stacking the insulating heat-conducting layer material, the electric heating material, the metal current-carrying strip and the insulating heat-insulating material in sequence, and then carrying out firing hot pressing in a vulcanizing machine to obtain the electric heating rubber composite material to be prepared. Wherein the temperature in the vulcanizing machine is 100 ℃ and the vulcanizing pressure is 5 MPa.
Example 7
Preparing oily conductive paste, comprising: 50 parts of polyvinyl butyral resin with an acetalization degree of 75% mol is weighed according to the mass and dissolved in 440 parts of dimethylformamide weighed according to the mass, then 10 parts of conductive carbon black weighed according to the mass and with the diameter of about 25 mu m is added, and finally, the conductive carbon black is ground for 30 minutes to be uniformly dispersed, so that the oily conductive slurry is obtained.
Preparing an electric heating material, comprising: bean curd cloth with the mesh number of 12 is selected as presoaked cloth to be immersed in the previously purchased oily conductive slurry, and mechanical stirring is carried out for 35min during immersion in order to ensure the uniformity of the immersion of the conductive slurry; taking out and flattening the prepreg cloth soaked with the conductive paste, and drying the prepreg cloth by an infrared dryer to obtain a material with electrothermal property; wherein, the content of the diluent after drying is ensured to be less than 1 percent during drying.
Preparing an insulating and heat-insulating layer material, comprising: mixing ethylene propylene diene monomer, methyl silicone oil, a vulcanizing agent, white carbon black, plasticizer and hollow alumina micro-beads (the diameter is 35 mu m) according to a proportion of 68: 7: 6: 5: 4: 10, and putting the mixture into a mixer for mixing; then banburying, rolling, cooling, warehousing and curing for 12 hours for later use.
Preparing an insulating heat-conducting layer material, comprising: mixing ethylene propylene diene monomer, methyl silicone oil, a vulcanizing agent, white carbon black, plasticization, aluminum nitride and silicon carbide according to the proportion of 63: 7: 6: 5: 4: 15, and putting the mixture into a mixer for mixing; then banburying, rolling, cooling, warehousing and curing for 9 hours for later use.
And stacking the insulating heat-conducting layer material, the electric heating material, the metal current-carrying strip and the insulating heat-insulating material in sequence, and then carrying out firing hot pressing in a vulcanizing machine to obtain the electric heating rubber composite material to be prepared. Wherein the temperature in the vulcanizing machine during vulcanization is 180 ℃, and the vulcanization pressure is 12 MPa.
Example 8
Preparing oily conductive paste, comprising: 150 parts of polyvinyl butyral resin with an acetalization degree of 85% mol is weighed according to the mass and dissolved in 300 parts of dimethylformamide weighed according to the mass, then 50 parts of conductive carbon black weighed according to the mass and with the diameter of about 25 mu m is added, and finally, the conductive carbon black is ground for 50 minutes to be uniformly dispersed, so that the oily conductive slurry is obtained.
Preparing an electric heating material, comprising: bean curd cloth with the mesh number of 20 is selected as presoaked cloth to be immersed in the prepared conductive slurry, and mechanical stirring is carried out for 30min during immersion in order to ensure the uniformity of the immersion of the conductive slurry; then taking out and flattening the prepreg cloth soaked with the conductive paste, and drying the prepreg cloth through an infrared dryer to obtain a material with electrothermal property; wherein, the content of the diluent after drying is ensured to be less than 1 percent during drying.
Preparing an insulating and heat-insulating layer material, comprising: mixing ethylene propylene diene monomer, methyl silicone oil, a vulcanizing agent, white carbon black, plasticization and hollow alumina micro-beads (the diameter is 60 mu m) according to a proportion of 65: 8: 6: 5: 4: 12, putting the mixture into a mixer for mixing; then banburying, rolling, cooling, warehousing and curing for 12 hours for later use.
Preparing an insulating heat-conducting layer material, comprising: mixing ethylene propylene diene monomer, methyl silicone oil, a vulcanizing agent, white carbon black, plasticization, aluminum nitride and silicon carbide according to the weight ratio of 57: 8: 6: 5: 4: weighing 20 parts by mass, and mixing in a mixer; then banburying, rolling, cooling, warehousing and curing for 16 hours for later use.
And stacking the insulating heat-conducting layer material, the electric heating material, the metal current-carrying strip and the insulating heat-insulating material in sequence, and then carrying out firing hot pressing in a vulcanizing machine to obtain the electric heating rubber composite material to be prepared. Wherein the temperature in the vulcanizing machine during vulcanization is 300 ℃, and the vulcanization pressure is 20 MPa.
The electric heating rubber obtained in the above embodiment has a three-layer structure as shown in fig. 1 and fig. 2, that is, an insulating heat conduction layer 1, an electric conduction heating layer 2 and an insulating heat insulation layer 3; the conductive heating layer is positioned between the insulating heat-conducting layer and the insulating heat-insulating layer. The conductive heating layer mainly comprises a netted flexible electric heating material 4 and a metal current carrying strip 5 which is arranged on the electric heating material 4 and used as an electrode.
The insulating and heat-insulating layer in the electric heating rubber is preferably hollow microspheres with the diameter of 10-100 mu m as heat-insulating filler, so that the blocking type heat-insulating material is prepared.
The electric heating rubber has the advantages that:
the electric heating rubber adopts the net-shaped flexible electric heating material as the conductive heating layer, and the conductive heating layer forms an even conductive network, so that the whole surface heating can be realized, the temperature is evenly distributed, and hot spots can not be formed for heating; this conductive heating layer embedding has strengthened whole electric heat rubber's intensity on the one hand in insulating rubber, and on the other hand makes it even through buckling the inflection, also can be because of the elasticity of rubber and the reconversion, has solved traditional electric heat rubber heating uneven and the problem that can't buckle many times.
Under the action of an electric field, carbon radicals in the conductive heating layer perform Brownian motion, violent friction and impact are generated among atoms, and the generated heat can be transmitted outwards in the form of infrared radiation, so that efficient electric-heat conversion is realized. Through the detection of a third party, the electrothermal radiation conversion efficiency reaches more than 90%, and compared with the traditional electrothermal mode, the electrothermal device is more energy-saving and power-saving.
The electric heating rubber is matt and noiseless, is the safest heating element known at present, and can greatly expand the application field of the electric heating rubber. The environment-friendly plastic can be applied to heating systems of building and transportation tools, is environment-friendly, non-toxic and harmless, has no pollution to the environment, does not contain radioactive elements, is quickly paved without cement and sand, can be paved by using environment-friendly special glue, and can be widely applied to large-scale public places such as rural coal-to-electricity, schools, hospitals, entertainment activities and the like, wherein the paving schematic diagram is shown in figure 3. In the industrial aspect: the heater can be applied to large-scale equipment preheating, oil pipelines and oil storage tanks. In the agricultural aspect: can be applied to incubator, greenhouse seedling raising and livestock shed heating and heat preservation. In the aspect of transportation: can be applied to ice and snow removal of airports, bridges and roads.
The electric heating rubber has the advantage of high heating speed. FIG. 4 shows that the resistance value of the electrothermal rubber is 10.7 omega, the pulse duty ratio is 1: after a voltage of 100 deg.C, the temperature of the electric heating rubber changes with the time of electrification, and it can be seen from the graph that the electric heating rubber can reach a higher temperature in about two minutes and then the temperature is basically kept stable.
The electric heating rubber has high reliability. The service life is one of important factors for measuring the quality, the processing efficiency and the cost of the electric heating rubber and is also an important index for measuring the manufacturing level of the electric heating rubber. If the service life of the electric heating rubber is low and the precision retentivity is poor, the cost of the product is greatly increased and the production efficiency is reduced. In order to examine the life and aging characteristics of the designed and manufactured electric heating rubber, the electric heating rubber of the present invention was subjected to a power-on test for a total of 500 hours, and fig. 5 is a change curve of resistance value measured with power-on time when the surface temperature of the electric heating rubber is room temperature: as can be seen from FIG. 5, the resistance value of the electric heating rubber conductive heating layer changes little from 10.7 Ω to 11 Ω within 500h of electrification, which has negligible influence on the heating rate and other properties of the whole electric heating rubber. Therefore, the electric heating rubber has high reliability, and does not have obvious aging phenomenon in the long-time electrifying process.
The electric heating rubber adopts a rubber vulcanization preparation process during preparation, and has the advantages of simple processing and low cost.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and are not limited. Although the present invention has been described in detail with reference to the embodiments, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (10)
1. The electric heating rubber is characterized by comprising an insulating heat conduction layer (1), a conductive heating layer (2) and an insulating and heat insulating layer (3), wherein the conductive heating layer (2) is positioned between the insulating heat conduction layer (1) and the insulating and heat insulating layer (3); wherein,
the conductive heating layer (2) is a flexible electric heating material with a conductive heating function, and a metal current carrying strip (5) serving as an electrode is arranged on the conductive heating layer (2).
2. The electric heating rubber according to claim 1, wherein the insulating and heat-insulating layer (3) adopts hollow microspheres with the diameter of 10-100 μm as heat-insulating filler.
3. The electric heating rubber according to claim 1, wherein the conductive heating layer (2) is in a grid shape with a mesh number in the range of 4-20 mesh to form a uniform conductive network.
4. A method for preparing an electrothermal rubber according to any one of claims 1 to 3, comprising:
immersing the prepreg cloth in the conductive coating, stirring and immersing, taking out the prepreg cloth with the conductive coating, flattening, and drying to obtain an electric heating material;
preparing an insulating material;
preparing an insulating heat conduction material;
stacking the insulating heat conduction material, the electric heating material, the metal current carrying strip and the insulating heat insulation material in sequence, and then carrying out firing hot pressing in a vulcanizing machine to obtain the electric heating rubber to be prepared; wherein the vulcanization temperature is between 100 and 300 ℃, and the vulcanization pressure is between 5 and 20 MPa.
5. The method for preparing electric heating rubber according to claim 4, wherein the conductive coating is a water-based conductive coating prepared by:
weighing 30-60% of waterborne polymer resin, adding 3-8% of coupling agent diluted by diluent, adding 5-40% of modified conductive filler into the waterborne polymer resin added with the coupling agent, and then grinding for 20-60 min to uniformly disperse the modified conductive filler to obtain waterborne conductive slurry; wherein,
the waterborne polymer resin adopts one or two of epoxy resin and polyimide; the diluent adopts one or two of acetone, MD212 and deionized water; the coupling agent is one or two of a ferrate coupling agent and a coupling agent KH 550; the conductive filler is one or two of graphite, carbon black, graphene and chopped carbon fiber.
6. The method for preparing electric heating rubber according to claim 4, wherein the conductive paint is oily conductive paint, and the oily conductive paint is prepared by:
weighing 10-30% of adhesive by mass, 60-90% of solvent by mass, dissolving the adhesive in the solvent, then weighing 2-10% of modified conductive filler, adding the conductive filler into the solvent in which the adhesive is dissolved, and finally grinding for 20-60 min to uniformly disperse the conductive filler to obtain oily conductive slurry; wherein,
the adhesive is polyvinyl butyral resin, the solvent is dimethylformamide, and the conductive filler is one or two of graphite, carbon black, graphene and chopped carbon fiber.
7. The preparation method of the electric heating rubber according to claim 4, wherein the pre-impregnated cloth is one of bean curd cloth and glass fiber mesh cloth, and the mesh number of the pre-impregnated cloth ranges from 4 meshes to 20 meshes.
8. The method of claim 4, wherein the preparing the insulating material comprises:
weighing 40-80% of ethylene propylene diene monomer, 5-10% of methyl silicone oil, 2-8% of vulcanizing agent, 3-6% of white carbon black, 3-5% of plasticizer and 5-15% of hollow microspheres according to the mass ratio, mixing in a mixer, banburying, rolling, cooling, warehousing and curing.
9. The method for preparing electrothermal rubber according to claim 8, wherein the cenospheres are cenospheres of hollow glass or cenospheres of hollow alumina.
10. The method for preparing electrothermal rubber according to claim 4, wherein preparing the insulating and heat-conducting material comprises:
weighing 30-75% of ethylene propylene diene monomer, 5-10% of methyl silicone oil, 2-8% of vulcanizing agent, 3-6% of white carbon black, 3-5% of plasticizer and 10-25% of high-thermal-conductivity filler according to the mass ratio, and mixing in a mixer; then banburying, rolling, cooling, warehousing and curing are carried out; wherein,
the high-thermal-conductivity filler is one or two of aluminum nitride and silicon carbide.
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| CN113248869A (en) * | 2021-05-12 | 2021-08-13 | 东北石油大学 | Carbon-series composite filler, high-thermal-conductivity electromagnetic shielding composite material and preparation method |
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Application publication date: 20190816 |