CN117410012B - Environment-friendly single-sided conductive foam and preparation process thereof - Google Patents
Environment-friendly single-sided conductive foam and preparation process thereof Download PDFInfo
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- CN117410012B CN117410012B CN202310999405.XA CN202310999405A CN117410012B CN 117410012 B CN117410012 B CN 117410012B CN 202310999405 A CN202310999405 A CN 202310999405A CN 117410012 B CN117410012 B CN 117410012B
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- 239000006260 foam Substances 0.000 title claims abstract description 92
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000000839 emulsion Substances 0.000 claims abstract description 65
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 59
- 229920002635 polyurethane Polymers 0.000 claims abstract description 58
- 239000004814 polyurethane Substances 0.000 claims abstract description 58
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims abstract description 54
- 238000005187 foaming Methods 0.000 claims abstract description 38
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 24
- 239000012948 isocyanate Substances 0.000 claims abstract description 23
- 150000002513 isocyanates Chemical class 0.000 claims abstract description 23
- 238000000576 coating method Methods 0.000 claims abstract description 22
- 239000000945 filler Substances 0.000 claims abstract description 22
- 239000000203 mixture Substances 0.000 claims abstract description 22
- 239000011248 coating agent Substances 0.000 claims abstract description 21
- 238000010438 heat treatment Methods 0.000 claims abstract description 20
- 239000002131 composite material Substances 0.000 claims abstract description 10
- 239000004088 foaming agent Substances 0.000 claims abstract description 10
- 239000011231 conductive filler Substances 0.000 claims abstract description 9
- 239000000758 substrate Substances 0.000 claims abstract description 7
- 229920005989 resin Polymers 0.000 claims description 70
- 239000011347 resin Substances 0.000 claims description 70
- 239000000843 powder Substances 0.000 claims description 44
- 229910052731 fluorine Inorganic materials 0.000 claims description 37
- 239000011737 fluorine Substances 0.000 claims description 37
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- 238000002156 mixing Methods 0.000 claims description 17
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- 239000002994 raw material Substances 0.000 claims description 15
- NBVXSUQYWXRMNV-UHFFFAOYSA-N fluoromethane Chemical compound FC NBVXSUQYWXRMNV-UHFFFAOYSA-N 0.000 claims description 14
- 239000007787 solid Substances 0.000 claims description 12
- 238000004519 manufacturing process Methods 0.000 claims description 11
- QTKPMCIBUROOGY-UHFFFAOYSA-N 2,2,2-trifluoroethyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OCC(F)(F)F QTKPMCIBUROOGY-UHFFFAOYSA-N 0.000 claims description 10
- JAHNSTQSQJOJLO-UHFFFAOYSA-N 2-(3-fluorophenyl)-1h-imidazole Chemical compound FC1=CC=CC(C=2NC=CN=2)=C1 JAHNSTQSQJOJLO-UHFFFAOYSA-N 0.000 claims description 10
- 239000003995 emulsifying agent Substances 0.000 claims description 10
- 150000002221 fluorine Chemical class 0.000 claims description 10
- 230000002209 hydrophobic effect Effects 0.000 claims description 10
- LVHBHZANLOWSRM-UHFFFAOYSA-N methylenebutanedioic acid Natural products OC(=O)CC(=C)C(O)=O LVHBHZANLOWSRM-UHFFFAOYSA-N 0.000 claims description 10
- 239000003999 initiator Substances 0.000 claims description 8
- 239000003973 paint Substances 0.000 claims description 7
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- 238000001816 cooling Methods 0.000 claims description 3
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- 125000001153 fluoro group Chemical group F* 0.000 claims description 2
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- ZHPNWZCWUUJAJC-UHFFFAOYSA-N fluorosilicon Chemical compound [Si]F ZHPNWZCWUUJAJC-UHFFFAOYSA-N 0.000 claims 1
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- -1 acrylic ester Chemical class 0.000 description 5
- 238000013329 compounding Methods 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000000853 adhesive Substances 0.000 description 3
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- KHXKESCWFMPTFT-UHFFFAOYSA-N 1,1,1,2,2,3,3-heptafluoro-3-(1,2,2-trifluoroethenoxy)propane Chemical compound FC(F)=C(F)OC(F)(F)C(F)(F)C(F)(F)F KHXKESCWFMPTFT-UHFFFAOYSA-N 0.000 description 1
- CDMDQYCEEKCBGR-UHFFFAOYSA-N 1,4-diisocyanatocyclohexane Chemical compound O=C=NC1CCC(N=C=O)CC1 CDMDQYCEEKCBGR-UHFFFAOYSA-N 0.000 description 1
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 1
- PTBDIHRZYDMNKB-UHFFFAOYSA-N 2,2-Bis(hydroxymethyl)propionic acid Chemical compound OCC(C)(CO)C(O)=O PTBDIHRZYDMNKB-UHFFFAOYSA-N 0.000 description 1
- 229910052582 BN Inorganic materials 0.000 description 1
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 239000004721 Polyphenylene oxide Substances 0.000 description 1
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical group [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 1
- 239000002390 adhesive tape Substances 0.000 description 1
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- 239000003063 flame retardant Substances 0.000 description 1
- 229920002313 fluoropolymer Polymers 0.000 description 1
- 239000004811 fluoropolymer Substances 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- IQPQWNKOIGAROB-UHFFFAOYSA-N isocyanate group Chemical group [N-]=C=O IQPQWNKOIGAROB-UHFFFAOYSA-N 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
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- 239000004417 polycarbonate Substances 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229920000570 polyether Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
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Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B5/00—Non-insulated conductors or conductive bodies characterised by their form
- H01B5/14—Non-insulated conductors or conductive bodies characterised by their form comprising conductive layers or films on insulating-supports
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K9/00—Screening of apparatus or components against electric or magnetic fields
- H05K9/0073—Shielding materials
- H05K9/0081—Electromagnetic shielding materials, e.g. EMI, RFI shielding
Abstract
The application relates to the field of conductive materials, in particular to environment-friendly single-sided conductive foam and a preparation process thereof. Comprising the following step 1): the preparation method comprises the steps of preparing a waterborne polyurethane acrylic emulsion, a conductive filler, an isocyanate curing agent, a foaming agent and an insulating filler, and respectively obtaining a conductive mixture, a foaming mixture and an insulating coating; 2): coating the coating mixture on a substrate, and heating and curing to form a conductive layer with the humidity of 62-68%; 3): coating the foaming mixture on a conductive layer, foaming to form a foaming layer, and obtaining a composite layer; 4): coating an insulating filler on another base material, curing to form an insulating layer with the humidity of 72-82%, preheating the composite layer, covering the insulating layer on the foaming layer, heating and curing, and tearing off the two base materials to obtain single-sided conductive foam; the foam has the advantages of good heat resistance, environmental protection, water resistance and the like.
Description
Technical Field
The application relates to the field of conductive materials, in particular to environment-friendly single-sided conductive foam and a preparation process thereof.
Background
The conductive foam is formed by wrapping conductive cloth on a flame-retardant sponge, and after a series of treatments, the conductive foam has good surface conductivity and can be easily fixed on a device to be shielded by using an adhesive tape. Shielding materials having different cross-sectional shapes, mounting methods, UL ratings and shielding effectiveness may be selected.
The conductive foam is very light in material, and can lead the electrostatic protection performance of the product to be permanent due to electromagnetic shielding performance. The material is light, so that the surface resistance capacity of the material is reduced, and the material has no dependence on the environmental humidity and the like. The conductive foam cloth has good corrosion resistance and oxidation resistance, so that the conductive foam cloth is widely applied to the fields of PDP televisions, LCD displays, liquid crystal televisions, mobile phones, notebook computers, MP3, communication cabinets, medical instruments, military industry, aerospace, new energy automobiles and the like.
The foam layer of the conductive foam is usually obtained by foaming solvent-type polyurethane resin, and the polyurethane resin is dissolved or needs to be diluted or dissolved by an organic solvent in the polymerization process, and the organic solvent is mostly easy to volatilize, so that a production workshop is polluted and the human health of workers is influenced.
For example, when the polyurethane foam is applied to the fields of medical instruments, military industry, aerospace, new energy automobiles and the like, the foam is easy to deform and age due to long-term high-temperature operation, so that the practicability of the polyurethane foam is reduced. Meanwhile, when the conductive foam is applied to a new energy battery of a new energy automobile, the new energy automobile is outdoor for a long time, and when the new energy automobile encounters heavy rain weather, the foam is easy to foam water or absorb moisture and the like, so that the layer structure of the foam is easy to fall off or the physical property and the heat conducting property of the foam are influenced, and therefore, the heat conducting foam needs to be further researched.
Disclosure of Invention
In order to solve the technical problems, the application provides an environment-friendly single-sided conductive foam and a preparation process thereof
In a first aspect, the present application provides a process for preparing environment-friendly single-sided conductive foam, which is characterized by comprising the following steps: 1): weighing 33-45 parts of aqueous polyurethane acrylic emulsion, 20-30 parts of conductive filler and 2.8-5.6 parts of isocyanate curing agent according to parts by weight, and uniformly mixing to obtain a conductive mixture for later use; weighing 30-50 parts of aqueous polyurethane acrylic emulsion, 3-8 parts of isocyanate curing agent and 0.1-0.8 part of foaming agent, and uniformly mixing to obtain a foaming mixture for later use; weighing 30-40 parts of aqueous polyurethane acrylic emulsion, 10-20 parts of insulating filler and 2-5 parts of isocyanate curing agent, and uniformly mixing to obtain insulating paint;
2): coating the coating mixture on a substrate, and heating and curing to form a conductive layer with the humidity of 62-68%;
3): coating the foaming mixture on a conductive layer, foaming to form a foaming layer, and obtaining a composite layer;
4): coating the insulating filler on another base material, curing to form an insulating layer with the humidity of 72-82%, preheating the composite layer, covering the insulating layer on the foaming layer, heating and curing, and tearing off the two base materials to obtain the single-sided conductive foam.
In the process, the single-sided conductive foam has the advantages of stable layer structure, good heat resistance, good water resistance and the like.
The polyurethane layer structure in the polyurethane foam is easy to expand when the polyurethane foam is soaked in water, and the performance of the polyurethane foam is influenced, because the polyurethane is a material formed by alternately arranging polyether or polyester chain segments and polyurethane chain segments, and ester bonds and ether bonds in the structure have certain sensitivity to moisture (the ester bonds and the ether bonds are polar groups and have hydrophilicity), so the polyurethane foam is easy to expand when the polyurethane foam is soaked in water, and the structure of the foam is fallen. Therefore, the conductive foam is prepared by taking the aqueous polyurethane acrylic emulsion as a main raw material.
The aqueous polyurethane acrylic emulsion is obtained by compounding water and polyurethane grafted acrylic emulsion in a weight ratio of 1:1, and the environment protection performance of the conductive foam is improved by taking water as a solvent, and the polyurethane grafted acrylic emulsion has strong cohesive force, good initial viscosity, high and low temperature resistance and the like by introducing special functional groups and special crosslinking monomers; the adhesive has better adhesive force and cohesive force on the adhesion, and a manufacturer can be preferably made by Nanjing sea new material science and technology limited company with the model number of 819; the viscosity at 25deg.C is 3000-5000CPS, and the solid content is 45-55%. Therefore, the aqueous polyurethane acrylic emulsion is used as the main raw material, so that the environment protection, high temperature resistance, water resistance and the like of the conductive foam can be further improved.
The isocyanate curing agent is a water-based closed isocyanate curing agent, the solid content is 40+/-1, and the NCO content is 4.8%; the viscosity at 25℃was 500 mPas. The aqueous polyurethane acrylic emulsion can be quickly unsealed at 120 ℃, can stably coexist with the aqueous polyurethane acrylic emulsion at normal temperature, can release isocyanate groups for reacting and crosslinking with hydroxyl, carboxyl, amino and other groups during heat sealing, and can obviously improve the performances of water resistance, chemical resistance, wear resistance, adhesive force, mechanical and mechanical properties and the like of the aqueous polyurethane acrylic emulsion. The conductive foam obtained by compounding the isocyanate curing agent with the aqueous polyurethane acrylic emulsion has better heat resistance, water resistance and the like.
The conductive filler has good conductivity, can enable the conductive mixture to have a conductive effect, and the foaming agent plays a role in foaming, so that a foam layer is formed conveniently. The insulating filler has an insulating effect.
The application can further improve the heat resistance, low temperature resistance, weather resistance and water resistance of the single-sided conductive foam by combining the aqueous polyurethane acrylic emulsion and the isocyanate curing agent, and reduce the possibility of influencing the performance of the single-sided conductive foam due to water absorption expansion.
In addition, the conductive filler, the insulating filler and the foaming agent are respectively added to obtain the layer structures with different performances. Thereby obtaining the single-sided conductive foam.
In summary, the application utilizes the combination of the aqueous polyurethane acrylic emulsion and the isocyanate curing agent with different additives to enhance the high temperature resistance, the water resistance and the like of the conductive foam, and is environment-friendly in the production process; when the insulating filler is added, the obtained insulating paint has a good insulating effect. In the step 2), the humidity of the conductive layer is enabled to be 62-68% in the curing process, so that the purpose is to enable the foaming layer to be stably bonded with the conductive layer, and the insulating layer humidity range (72-82%) in the step 4) is convenient for the stable bonding of the insulating layer and the foam layer, and the composite layer is preheated, so that the bonding stability of the insulating layer and the foam layer is further improved. When the conductive foam is used in a new energy automobile, the possibility that the conductive foam bubbles, falls off and the like after the new energy automobile bubbles is reduced, and the possibility that water absorption and moisture absorption occur in the using process is also reduced.
If the insulating layer is completely solidified and then combined with the foam layer, unstable adhesion can be caused; if the insulating filler is directly coated on the foam layer in a coating mode, the foam layer contains a large number of pores, and the surface is uneven, so that the thickness of the insulating layer formed by the film is difficult to control in the coating process, and part of pores can be blocked, so that the performance of the foam is affected.
Because the raw material systems of the insulating layer, the foam layer and the conductive layer all contain the polyurethane acrylic emulsion and the isocyanate curing agent, the layer structure is easy to adhere and stable, the possibility of falling off of the layer structure is reduced, and the possibility of water absorption expansion of the single-sided conductive foam is further reduced.
Preferably, the curing temperature in both 2) and 4) is 100-120 ℃; the 3) foaming temperature is 110-130 ℃ and the foaming time is 5-10min; the preheating temperature in the step 4) is 80-90 ℃ and the preheating time is 10-20s.
The adoption of the curing temperature in the range is convenient for forming the conductive layer, the foaming layer, the insulating layer and the like, and the foaming temperature and the foaming time ensure that the foaming of the foam layer is stable, and the formed foam is stable. The preheating temperature and time can further improve the bonding stability of the insulating layer and the foaming layer.
Preferably, the aqueous polyurethane acrylic emulsion comprises the following raw materials in parts by weight:
50-80 parts of polyurethane grafted acrylic emulsion
50-80 parts of water
EAA emulsion 1-5 parts
3-8 parts of temperature-resistant hydrophobic filler;
the temperature-resistant hydrophobic filling is fluorine-containing resin powder.
A thermoplastic resin containing fluorine atoms in the molecular structure of fluorine-containing resin powder. Has excellent high and low temperature resistance, chemical stability, weather resistance, incombustibility, hydrophobicity, etc. Therefore, the temperature-resistant hydrophobic filler has better hydrophobicity and heat resistance. The EAA emulsion has good adhesion, can further improve the adhesion of the aqueous polyurethane acrylic emulsion, and simultaneously ensures that the fluororesin powder is stably adhered to a raw material system. Further improves the hydrophobicity, heat resistance, weather resistance and adhesiveness of the aqueous polyurethane acrylic emulsion after film formation. The obtained conductive foam has stable layer structure, hydrophobicity, heat resistance and the like.
Preferably, the mesh number of the fluorine-containing resin powder is 300 to 1000 mesh.
The selection of the above mesh can lead the fluorine-containing resin powder to be uniformly dispersed in the aqueous polyurethane acrylic emulsion. The fluorine-containing resin powder of the present application is used as a filler, and only plays a role in filling, and does not react or dissolve. The heat resistance and the hydrophobicity of the single-sided conductive foam can be further improved.
Preferably, the fluorine-containing resin powder is a compatibility-modified fluorine-containing resin powder.
The modified fluorine-containing resin powder can further improve the dispersion uniformity of the fluorine-containing resin powder in the aqueous polyurethane acrylic emulsion and further improve the hydrophobicity and the heat resistance of the single-sided conductive foam.
Preferably, the compatibility-modified fluororesin powder is prepared from the following raw materials in parts by weight:
16-25 parts of fluorine-containing resin powder
Initiator 0.1-0.8 part
0.5-1 part of emulsifying agent
20-32 parts of water
3-8 parts of itaconic acid
1-5 parts of trifluoroethyl methacrylate.
Preferably, the compatibility-modified fluororesin powder is prepared by the steps of:
weighing itaconic acid, trifluoroethyl methacrylate, an emulsifier, water and an initiator according to parts by weight, uniformly mixing, heating to 75-95 ℃, reacting for 30-60min, neutralizing, adding fluorine-containing resin powder, stirring for 10-30min at the rotating speed of 120-180r/min, filtering, drying, heating the obtained solid to 280-320 ℃, stirring for 10-20min, cooling, and crushing to obtain compatibility modified fluorine-containing resin powder.
Itaconic acid is an acrylic ester monomer of unsaturated dibasic organic acid, has better water resistance and heat resistance after being polymerized with trifluoroethyl methacrylate, and can improve weather resistance, water resistance and pollution resistance, and is easy to be compatible with fluorine-containing resin powder due to containing fluorine ions.
The fluorine-containing resin is generally a nonpolar material, and the surface of the fluorine-containing resin is waxy and presents hydrophobicity, temperature resistance and the like, so that the fluorine-containing resin is compounded by itaconic acid and trifluoroethyl methacrylate, and under the auxiliary action of an emulsifying agent, an initiating agent and an alcohol solution, a compound macromolecular acrylic ester emulsion is formed, and fluorine-containing resin powder is added to make the fluorine-containing resin compatible with the fluorine-containing resin powder. The obtained solid is heated, melted and blended after being filtered and dried, so that compatibility modified fluorine-containing resin powder is obtained, the fluorine-containing resin powder has a good dispersing effect, can be uniformly dispersed in aqueous polyurethane acrylic emulsion, is tightly combined with raw materials of a system after being solidified and formed into a film, and further improves heat resistance, hydrophobicity, water resistance and the like of single-sided conductive foam.
Preferably, the fluorine-containing resin is one or more of fluorocarbon resin, fluorosilicone resin and PFA.
Fluorocarbon resins are a type of fluoropolymer material that is a copolymer made by reacting a fluoromonomer with an epoxy resin or carbonyl compound. The fluorocarbon resin has the characteristics of high thermal stability, high chemical stability, excellent high temperature resistance, excellent chemical corrosion resistance and the like. In addition, the fluorocarbon resin has very low surface tension, excellent anti-sticking performance, small interaction force with water molecules and hydrophobicity. Therefore, the fluorocarbon resin can further improve the heat resistance and the hydrophobicity of the single-sided conductive foam.
The fluorosilicone resin, also called fluorosilicone copolymer resin, is a synthetic resin obtained by mixing a fluororesin and an organic silicone resin, and has excellent temperature resistance, hydrophobicity, antifouling property and the like.
PFA is a copolymer of a small amount of perfluoropropyl perfluorovinyl ether and polytetrafluoroethylene. Has better temperature resistance, hydrophobicity, antifouling property and other fluorine-containing resins.
Therefore, the fluorine-containing resin with one or more of the above compositions can further improve the heat resistance, the hydrophobicity and the water resistance of the single-sided conductive foam.
Preferably, the ratio of the fluorocarbon resin, the fluorosilicone resin and the PFA in parts by weight is 1: (0.3-0.5) and (0.1-0.3).
When fluorocarbon resin, fluorosilicone resin and PFA are compounded, the synergistic effect is achieved, so that the single-sided conductive foam is better in heat resistance, water resistance and hydrophobicity.
Preferably, the aqueous polyurethane acrylic emulsion is prepared by the following steps: and (3) weighing the polyurethane grafted acrylic emulsion, water, the EAA emulsion and the temperature-resistant hydrophobic filler according to parts by weight, and uniformly mixing to obtain the aqueous polyurethane acrylic emulsion.
The preparation method is simple to operate, the conductive foam is obtained by mixing and stirring at normal temperature, water is used as a solvent, the conductive foam is more environment-friendly in the production process, and the obtained conductive foam has the advantages of good heat resistance, hydrophobicity, water resistance and the like, and the possibility of water absorption expansion or moisture absorption during use is reduced. Can also be used for high-heating products such as new energy automobiles.
In a second aspect, the application provides an environment-friendly single-sided conductive foam, which sequentially comprises a conductive layer, a foam layer and an insulating layer from the upper surface to the lower surface, and is characterized in that the environment-friendly single-sided conductive foam is prepared by adopting a preparation process of the environment-friendly single-sided conductive foam.
In summary, the present application has the following beneficial effects:
1. the water-based polyurethane acrylic emulsion, the isocyanate curing agent and different additives are combined, so that the high temperature resistance, the water resistance and the like of the conductive foam are enhanced, and the production process is environment-friendly; when the insulating filler is added, the obtained insulating paint has a good insulating effect. In the step 2), the humidity of the conductive layer is enabled to be 62-68% in the curing process, so that the purpose is to enable the foaming layer to be stably bonded with the conductive layer, and the insulating layer humidity range (72-82%) in the step 4) is convenient for the stable bonding of the insulating layer and the foam layer, and the composite layer is preheated, so that the bonding stability of the insulating layer and the foam layer is further improved. When the conductive foam is used in a new energy automobile, the possibility that the conductive foam bubbles, falls off and the like after the new energy automobile bubbles is reduced, and the possibility that water absorption and moisture absorption occur in the using process is also reduced.
2. The preparation method comprises the steps of compounding itaconic acid and trifluoroethyl methacrylate, forming a compound macromolecular acrylic ester emulsion under the auxiliary action of an emulsifier, an initiator and an alcohol solution, and adding fluorine-containing resin powder to enable the emulsion to be compatible with the fluorine-containing resin powder. The obtained solid is heated, melted and blended after being filtered and dried, so that compatibility modified fluorine-containing resin powder is obtained, the fluorine-containing resin powder has a good dispersing effect, can be uniformly dispersed in aqueous polyurethane acrylic emulsion, is tightly combined with raw materials of a system after being solidified and formed into a film, and further improves heat resistance, hydrophobicity, water resistance and the like of single-sided conductive foam.
3. The fluorocarbon resin, the fluorosilicone resin and the PFA are compounded to play a synergistic effect, so that the single-sided conductive foam is better in heat resistance, water resistance and hydrophobicity.
Detailed Description
The present application is described in further detail below with reference to examples.
Partial sources of raw materials:
fluorocarbon resin with number average molecular weight of 20000-30000 and fluorine content of 20.1-22.3%;
the manufacturer of the fluorosilicone resin is DOW fluorosilicone resin SILASTIC FL-9201 of Tao Shitao;
the brand of PFA is Japanese Dajin, the brand number is AP-230;
the model of the new material science and technology Co., ltd of Nanjing Tianshi of EAA emulsion manufacturer is OE-7013;
the foaming agent is preferably microsphere foaming agent, and the brand is UNICCELL, and the model is PG07;
the emulsifier is preferably sodium dodecyl sulfate;
the conductive filler is 500-mesh graphene;
the insulating filler is 300 mesh hexagonal boron nitride.
Examples
Example 1
An environment-friendly single-sided conductive foam sequentially comprises a conductive layer, a foam layer and an insulating layer from the upper surface to the lower surface.
The preparation of the environment-friendly single-sided conductive foam comprises the following steps:
1): weighing 3.3kg of aqueous polyurethane acrylic emulsion, 2kg of conductive filler and 0.28kg of isocyanate curing agent according to parts by weight, and uniformly mixing to obtain a conductive mixture for later use; weighing 3kg of aqueous polyurethane acrylic emulsion, 0.3kg of isocyanate curing agent and 0.01kg of foaming agent, and uniformly mixing to obtain a foaming mixture for later use; weighing 3kg of aqueous polyurethane acrylic emulsion, 1kg of insulating filler and 0.2kg of isocyanate curing agent, and uniformly mixing to obtain insulating paint;
2): coating the coating mixture on a PET substrate with a coating weight of 30g/m 2 Heating and solidifying to form a conductive layer with the humidity of 62%;
3): coating the foaming mixture on the conductive layer with the coating weight of 60g/m 2 Foaming to form a foaming layer to obtain a composite layer;
4): coating an insulating filler on another PET substrate with a coating weight of 30g/m 2 And curing until an insulating layer with the humidity of 80% is formed, preheating the composite layer, covering the insulating layer on the foaming layer, extruding by double rollers, wherein the pressure is 5N, so that the insulating layer is fully contacted with the foaming layer, and simultaneously, heating and curing to further cure the insulating layer, tearing off the two first base materials and the second base materials, thereby obtaining the single-sided conductive foam.
Wherein the curing temperature in both 2) and 4) is 100 ℃; 3) The foaming temperature is 110 ℃, and the foaming time is 8min; 4) The preheating temperature is 85 ℃ and the preheating time is 15s.
The aqueous polyurethane acrylic emulsion is obtained by compounding water and polyurethane grafted acrylic emulsion according to the weight (kg) ratio of 1:1, the viscosity at 25 ℃ is 3000CPS, and the solid content is 50%.
Example 2
Example 2 differs from example 1 in the amount of raw materials used, specifically as follows;
conductive mixture: 4.0kg of aqueous polyurethane acrylic emulsion, 2.5kg of conductive filler and 0.42kg of isocyanate curing agent;
foaming mixture: 4kg of aqueous polyurethane acrylic emulsion, 0.5kg of isocyanate curing agent and 0.05kg of foaming agent;
insulating paint: 3.5kg of aqueous polyurethane acrylic emulsion, 1.5kg of insulating filler and 0.4kg of isocyanate curing agent.
Example 3
Example 3 differs from example 1 in the amount of raw materials used, specifically as follows;
conductive mixture: 4.5kg of aqueous polyurethane acrylic emulsion, 3kg of conductive filler and 0.56kg of isocyanate curing agent;
foaming mixture: 5kg of aqueous polyurethane acrylic emulsion, 0.8kg of isocyanate curing agent and 0.08kg of foaming agent;
insulating paint: 4kg of aqueous polyurethane acrylic emulsion, 2kg of insulating filler and 0.5kg of isocyanate curing agent.
Example 4
Example 4 differs from example 2 in that the aqueous polyurethane acrylic emulsion is prepared by the following steps: pulverizing fluorocarbon resin, and sieving with 500 mesh sieve to obtain fluorine-containing resin powder; weighing 5kg of polyurethane grafted acrylic emulsion, 5kg of water, 0.1kg of EAA emulsion and 0.3kg of fluorine-containing resin powder, and uniformly mixing to obtain the aqueous polyurethane acrylic emulsion.
Example 5
Example 5 is different from example 4 in that the fluorine-containing resin powder is composed of fluorocarbon resin, fluorosilicone resin, PFA in a weight (kg) ratio of 1:0.3:0.2, and placing into a pulverizer for pulverizing, and sieving with 500 mesh sieve.
Example 6
Example 6 is different from example 5 in that the fluorine-containing resin powder is a compatibility-modified fluorine-containing resin powder, which is produced by the steps of:
weighing 2kg of itaconic acid, 1kg of trifluoroethyl methacrylate, 0.5kg of emulsifying agent, 20kg of water and 0.1kg of initiator, uniformly mixing, heating to 80 ℃, reacting for 40min, adding a sodium hydroxide solution with the mass fraction of 5% to neutralize to pH 7, adding 16kg of fluorine-containing resin powder, stirring for 20min at the rotating speed of 150r/min, filtering, drying the solid filter residue, heating the obtained solid to 300 ℃, stirring for 20min at the rotating speed of 100r/min, cooling to 30min, crushing, sieving for 500 meshes, and obtaining compatibility modified fluorine-containing resin powder.
Example 7
Example 7 differs from example 6 in that: 5kg of itaconic acid, 3kg of trifluoroethyl methacrylate, 0.8kg of emulsifier, 25kg of water, 0.5kg of initiator and 20kg of fluororesin powder.
Example 8
Example 8 differs from example 6 in that: 8kg of itaconic acid, 5kg of trifluoroethyl methacrylate, 1kg of an emulsifier, 30kg of water, 0.8kg of an initiator, and 32kg of a fluororesin powder.
Comparative example
Comparative example 1
Comparative example 1 differs from example 1 in that: the aqueous polyurethane acrylic emulsion is aqueous polyurethane solution (viscosity at 25 ℃ C. Is 3000CPS, solid content is 50%, and main raw materials comprise polytetrahydrofuran dihydric alcohol, polycarbonate dihydric alcohol, 1, 4-cyclohexane diisocyanate and dimethylolpropionic acid).
Performance test
The single-sided conductive foam obtained in examples 1 to 8 and comparative example 1 was subjected to the following performance test, as shown in table 1.
Detection method/test method
1. Hydrophobic and Water resistance test
1) And (3) water resistance test: the single-sided conductive foam obtained in examples 1 to 8 and comparative example 1 was completely immersed in water at 25 ℃ for 1 day, taken out, and whether the conductive layer and the insulating layer were bulged or cracked was observed, and if the above phenomenon was not qualified, and the related data were recorded in table 1.
2) Water absorption rate: cutting the single-sided conductive foam obtained in examples 1-8 and comparative example 1 into 10cm x 10cm test samples, and weighing and recording as W1; then the humidity of the test sample is 85%, the temperature is 40 ℃ for 1h, the weighing weight is recorded as W1, the water absorption rate is = [ (W2-W1)/W1 ]100%, and specific data are shown in table 1;
3) Contact angle: with reference to the national standard GB/T30047-2013, θ represents the contact angle, when 0 < θ < 90 °, the liquid wets the solid, and the smaller the wetting property is, the better. Called hydrophilic contact angle. The liquid does not wet the solid, and theta is more than 90 DEG and less than 180 deg. Also called hydrophobic contact angle, or hydrophobic contact angle; and (3) detecting the contact angle by dropping water on the surface of the conductive layer.
2. Heat resistance test
The single-sided conductive foam obtained in examples 1 to 8 and comparative example 1 was cut into 10cm x 10cm samples, one side of the conductive layer was adhered to 200g of glass plate by double-sided tape, and one side of the insulating layer was adhered to another 200g of glass plate by double-sided tape, to obtain test samples, and the height of the test samples was measured and recorded as h; placing the test sample in an oven at 120 ℃ for 24 hours (humidity of 50%), wherein a glass plate of an insulating layer of the test sample is contacted with the bottom of the oven, and detecting the height of the test sample to be h1 after recording and heating for 24 hours; and the blank group, the test sample is placed in an environment with the temperature of 25 ℃ and the humidity of 50% for 24 hours, wherein one glass plate of an insulating layer of the test sample faces downwards (contacts with a placing table surface), and the height of the test sample is detected to be h2. Calculating the compression change rate= [ (h-h 2)/h ]%; the rate of change of temperature= [ (h-h 1)/h ]%; the heating change rate=the heating change rate-the compression change rate, and when the heating change rate is large, the heat stability of the foam is poor;
table 1 experimental data for examples 1-8 and comparative example 1
| Test item | Water resistance | Water absorption (%) | Contact angle (°) | Rate of change by heat (%) |
| Example 1 | Qualified product | 2.87 | 105 | 2.79 |
| Example 2 | Qualified product | 2.72 | 108 | 2.71 |
| Example 3 | Qualified product | 2.73 | 108 | 2.64 |
| Example 4 | Qualified product | 1.61 | 118 | 2.03 |
| Example 5 | Qualified product | 1.27 | 125 | 1.82 |
| Example 6 | Qualified product | 0.98 | 128 | 1.36 |
| Example 7 | Qualified product | 0.85 | 130 | 1.08 |
| Example 8 | Qualified product | 0.84 | 129 | 1.11 |
| Comparative example 1 | Failure to pass | 4.68 | 93 | 10.65 |
As can be seen by combining example 1 and comparative example 1 and combining the tables, example 1 is a bubbling phenomenon, whereas comparative example 1 is a bubbling phenomenon; meanwhile, the water absorption rate and the heating change rate of the conductive foam are lower than those of the comparative example 1, the contact angle is higher than that of the comparative example 1, and the environment friendliness, heat resistance, water resistance and the like of the conductive foam can be further improved by adopting the aqueous polyurethane acrylic emulsion as a main raw material.
Comparing example 1 with example 4, it can be seen that the water absorption and heat resistance change rate of example 4 are lower than those of example 1, and the contact angle is higher than that of example 1, which indicates that the prepared conductive foam has better hydrophobicity, water resistance, heat resistance and the like by the aqueous polyurethane acrylic emulsion obtained by compounding the polyurethane grafted acrylic emulsion, fluorine-containing resin powder and EAA emulsion.
Comparing example 4 with example 5, it can be seen that the water absorption and heat resistance change rate of example 5 are lower than those of example 4, and the contact angle is higher than that of example 4, so that the synergistic effect can be achieved when fluorocarbon resin, fluorosilicone resin and PFA are used in combination, and the conductive foam can obtain better hydrophobicity, water resistance, heat resistance and the like.
As can be seen from the comparison of examples 5 and 6, the water absorption and heat resistance change rate of example 6 are lower than those of example 5, and the contact angle is higher than that of example 5, and when the compatibility-modified fluororesin powder is used, the compatibility with the polymer is further improved, and the conductive foam has better hydrophobicity, water resistance, heat resistance and the like.
The present embodiment is merely illustrative of the present application and is not intended to be limiting, and those skilled in the art, after having read the present specification, may make modifications to the present embodiment without creative contribution as required, but is protected by patent laws within the scope of the claims of the present application.
Claims (8)
1. The preparation process of the environment-friendly single-sided conductive foam is characterized by comprising the following steps of:
1): weighing 33-45 parts of aqueous polyurethane acrylic emulsion, 20-30 parts of conductive filler and 2.8-5.6 parts of isocyanate curing agent according to parts by weight, and uniformly mixing to obtain a conductive mixture for later use; weighing 30-50 parts of aqueous polyurethane acrylic emulsion, 3-8 parts of isocyanate curing agent and 0.1-0.8 part of foaming agent, and uniformly mixing to obtain a foaming mixture for later use; weighing 30-40 parts of aqueous polyurethane acrylic emulsion, 10-20 parts of insulating filler and 2-5 parts of isocyanate curing agent, and uniformly mixing to obtain insulating paint;
2): coating the conductive mixture on a substrate, and heating and curing to form a conductive layer with the humidity of 62-68%;
3): coating the foaming mixture on a conductive layer, foaming to form a foaming layer, and obtaining a composite layer;
4): coating an insulating coating on another substrate, curing to form an insulating layer with the humidity of 72-82%, preheating the composite layer, covering the insulating layer on the foaming layer, heating and curing, and tearing off the two substrates to obtain single-sided conductive foam;
the aqueous polyurethane acrylic emulsion comprises the following raw materials in parts by weight:
50-80 parts of polyurethane grafted acrylic emulsion
50-80 parts of water
EAA emulsion 1-5 parts
3-8 parts of temperature-resistant hydrophobic filler;
the temperature-resistant hydrophobic filler is fluorine-containing resin powder;
the fluorine-containing resin powder is compatibility modified fluorine-containing resin powder, and the compatibility modified fluorine-containing resin powder is prepared from the following raw materials in parts by weight:
16-25 parts of fluorine-containing resin powder
Initiator 0.1-0.8 part
0.5-1 part of emulsifying agent
20-32 parts of water
3-8 parts of itaconic acid
1-5 parts of trifluoroethyl methacrylate.
2. The process for preparing the environment-friendly single-sided conductive foam according to claim 1, which is characterized in that: the curing temperature in the steps 2) and 4) is 100-120 ℃; the 3) foaming temperature is 110-130 ℃ and the foaming time is 5-10min; the preheating temperature in the step 4) is 80-90 ℃ and the preheating time is 10-20s.
3. The process for preparing the environment-friendly single-sided conductive foam according to claim 1, which is characterized in that: the mesh number of the fluorine-containing resin powder is 300-1000 mesh.
4. The process for preparing environment-friendly single-sided conductive foam according to claim 1, wherein the compatibility-modified fluororesin powder is prepared by the following steps:
weighing itaconic acid, trifluoroethyl methacrylate, an emulsifier, water and an initiator according to parts by weight, uniformly mixing, heating to 75-95 ℃, reacting for 30-60min, neutralizing, adding fluorine-containing resin powder, stirring for 10-30min at the rotating speed of 120-180r/min, filtering, drying, heating the obtained solid to 280-320 ℃, stirring for 10-20min, cooling, and crushing to obtain compatibility modified fluorine-containing resin powder.
5. The process for preparing the environment-friendly single-sided conductive foam according to claim 1, which is characterized in that: the fluorine-containing resin is one or more of fluorocarbon resin, fluorine silicon resin and PFA.
6. The process for preparing the environment-friendly single-sided conductive foam according to claim 5, which is characterized in that: the fluorocarbon resin, the fluorosilicone resin and the PFA are mixed according to the weight ratio of 1: (0.3-0.5) and (0.1-0.3).
7. The process for preparing the environment-friendly single-sided conductive foam according to claim 1, wherein the aqueous polyurethane acrylic emulsion is prepared by the following steps: and (3) weighing the polyurethane grafted acrylic emulsion, water, the EAA emulsion and the temperature-resistant hydrophobic filler according to parts by weight, and uniformly mixing to obtain the aqueous polyurethane acrylic emulsion.
8. An environment-friendly single-sided conductive foam sequentially comprises a conductive layer, a foam layer and an insulating layer from the upper surface to the lower surface, and is characterized in that the environment-friendly single-sided conductive foam is prepared by adopting the preparation process of any one of claims 1-7.
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