CN112721382A - Composite film - Google Patents
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- CN112721382A CN112721382A CN202110112486.8A CN202110112486A CN112721382A CN 112721382 A CN112721382 A CN 112721382A CN 202110112486 A CN202110112486 A CN 202110112486A CN 112721382 A CN112721382 A CN 112721382A
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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
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/36—Layered products comprising a layer of synthetic resin comprising polyesters
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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
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/06—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B27/08—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
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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
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/28—Layered products comprising a layer of synthetic resin comprising synthetic resins not wholly covered by any one of the sub-groups B32B27/30 - B32B27/42
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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
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/34—Layered products comprising a layer of synthetic resin comprising polyamides
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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
- B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
- B32B7/04—Interconnection of layers
- B32B7/10—Interconnection of layers at least one layer having inter-reactive properties
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
- C08L77/10—Polyamides derived from aromatically bound amino and carboxyl groups of amino-carboxylic acids or of polyamines and polycarboxylic acids
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J175/00—Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
- C09J175/04—Polyurethanes
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
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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
- B32B2307/20—Properties of the layers or laminate having particular electrical or magnetic properties, e.g. piezoelectric
- B32B2307/206—Insulating
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
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- Laminated Bodies (AREA)
- Organic Insulating Materials (AREA)
Abstract
The invention provides an insulating material with excellent aging resistance, good insulation property, good rigidity, simple processing method and low cost, which is provided with one or more polymer film layers and one or more adhesive layers, wherein after the composite film is subjected to oil aging tests for 4 times, the breaking strength retention rate is more than 50%, the breaking elongation retention rate is more than 53%, and the peel strength is more than 1N/cm, at least one of the polymer film layers is a polyphenylene sulfide film layer, and the composite film contains an aramid fiber paper layer.
Description
The application is a divisional application of an invention application with application date of 2017, 1, 17 and application number of 201710033822.3 and the name of composite film.
Technical Field
The invention belongs to the field of high polymer materials, and relates to a multilayer composite film.
Background
In recent years, with the progress of new energy vehicles such as hybrid vehicles and electric vehicles, electric motors have been becoming smaller, higher in output, and higher in reliability. An insulating film (or insulating paper) is used for insulation between the coil and the core, and there is also a strong demand for high performance. In particular, certain oil-cooled (or oil-immersed) motors, in their operating state, the coils, the core and its insulating film are immersed in the automatic transmission oil. Therefore, when the insulating film is used in such a motor, it is required to have excellent properties such that the mechanical properties and the insulating properties thereof do not change significantly even after being soaked in a transmission oil having a small amount of water alternating between high and low temperatures for a long period of time.
At present, the following insulating films are known to be used in electric motors of new energy vehicles:
1. aromatic polyamide paper, i.e. aramid paper, such as the product of dupont, usa under the trade name Nomex (Nomex). The paper has general oil resistance and hydrolysis resistance, and when used in an oil-cooled motor, the paper has problems of reduced elongation at break and increased brittleness. The rigidity is poor, and the actual processing requirement is difficult to adapt to sometimes. Further, since it is a paper material, the insulation property is also poor.
2. The biaxially stretched polyphenylene sulfide (PPS) film has excellent oil resistance and hydrolysis resistance, but is limited by the preparation method thereof, and the single layer PPS film has a small thickness and insufficient rigidity to be used in an insulation film. Japanese patent application laid-open No. 2-45144 proposes a laminate film obtained by heat-fusing a PPS film and an unstretched PPS sheet as a laminate film for electrical insulation used in the field of electric motors. However, the film obtained by this proposal has low interlayer adhesiveness, and therefore, delamination and cracks are generated due to stress concentration during processing and use.
CN 201080028738.9 provides a composite material solution, after the surface of at least one material of aramid fiber paper and PPS film is processed by low-temperature plasma, the composite material, NSN for short, is prepared by directly pressing and laminating without using adhesive. The composite material has better oil resistance and hydrolysis resistance, but has the following defects: the equipment and the composite process for low-temperature plasma treatment are complex, the production period is too long, the cost is high, and the low-temperature plasma treatment equipment is not suitable for large-scale production; in the treatment process, the material has the possibility of electrostatic charge, so that the reliability of the service performance is influenced; brittle and easily broken during processing.
4. Composite films of aramid paper and polyethylene terephthalate (PET), polyethylene naphthalate (PEN), Polyimide (PI) films are abbreviated as NMN, NPN, NHN, respectively. Although the oil-resistant PET, PEN and PI have the advantage of simple processing, the mechanical properties of the PET, PEN and PI are remarkably reduced and even broken in the oil aging test process due to the poor oil resistance of the PET, PEN and PI, so that the oil-resistant PET, PEN and PI can not be suitable for oil-cooled motors.
Therefore, there is still a need for a high-performance insulating film with excellent aging resistance, good insulation, good rigidity, simple processing method and low cost, so as to meet the development trend of new energy vehicles, especially the application requirement of oil-cooled motors.
Disclosure of Invention
The invention aims to provide an insulating film which has excellent aging resistance, good insulating property, good rigidity, simple processing method and low cost and is particularly suitable for an oil-cooled motor.
The present inventors have conducted intensive studies to solve the above problems, and as a result, have found that a composite film comprising one or more polymer film layers and one or more adhesive layers, which has a fracture strength retention ratio of more than 50% and a peel strength of more than 1N/cm after an oil aging test conducted 4 cycles, can solve the above problems. Preferably, the breaking strength retention is greater than 70% and the peel strength is greater than 1.5N/cm.
The present invention provides the following aspects.
(1) A composite film characterized by: the composite film is provided with one or more polymer film layers and one or more adhesive layers, and after the composite film is subjected to an oil aging test for 4 times, the fracture strength retention rate is more than 50%, and the peel strength is more than 1N/cm.
(2) The composite film according to (1), characterized in that: after the composite film is subjected to an oil aging test for 4 times, the breaking elongation retention rate is more than 30%, and the insulation breakdown voltage is more than 8 kV.
(3) The composite film according to (1), characterized in that: after the composite film is subjected to an oil aging test for 8 times, the fracture strength retention rate is more than 50%, and the peel strength is more than 1N/cm.
(4) The composite film according to (2), characterized in that: after the composite film is subjected to an oil aging test for 8 times, the breaking elongation retention rate is more than 30%, and the insulation breakdown voltage is more than 8 kV.
(5) The composite film according to (1), characterized in that: after the composite film is subjected to a damp-heat aging experiment, the breaking strength retention rate is more than 80%, the breaking elongation retention rate is more than 70%, the peeling strength is more than 1N/cm, and the dielectric breakdown voltage is more than 8 kV.
(6) The composite film according to any one of (1) to (5), characterized in that: at least one layer of the polymer film layer is a polyphenylene sulfide film layer, and the composite film contains an aramid paper layer.
(7) The composite film according to (6), characterized in that: at least one layer of the polymer film layers is a two-way stretching polyphenylene sulfide film layer.
(8) The composite film according to (1), characterized in that: the adhesive is one or more of epoxy, polyurethane, acrylic or organosilicon adhesives.
(9) The composite film according to (1), characterized in that: the breaking strength of the composite film is more than 120MPa, the peeling strength is more than 2N/cm, and the dielectric breakdown voltage is more than 10 kV.
(10) The composite film according to (1), characterized in that: after the composite film is subjected to an oil aging test for 8 times, the breaking strength is greater than 80MPa, and the breaking elongation is greater than 10%.
In general, the mechanical properties of the composite film in the Machine Direction (MD) and Transverse Direction (TD) are not necessarily the same. Unless otherwise specified, the mechanical properties of the composite film referred to herein refer to the mechanical properties in the MD direction thereof.
Further, considering that the material needs to maintain toughness to some extent, the composite film preferably has an elongation at break retention ratio of more than 30% and a dielectric breakdown voltage of more than 8kV after 4 cycles of an oil aging test. When the elongation at break retention is less than 30%, the material may be too brittle and may be broken during use. When the dielectric breakdown voltage is less than 8kV, the dielectric properties of the material may deteriorate, and the dielectric effect may not be exhibited in the use process. Further preferably, the elongation at break retention ratio is more than 50%, and the dielectric breakdown voltage is more than 10 kV.
The oil aging test is a cyclic aging test in which a sample is immersed in a mixed liquid consisting of 99.5 vol% of automatic transmission oil and 0.5 vol% of water, the temperature is raised from room temperature to 155 ℃ at a rate of about 2 ℃/min and then isothermal for 40 hours, then the temperature is lowered to-45 ℃ at a rate of about 2 ℃/min and then isothermal for 8 hours, and then the temperature is raised to room temperature at a rate of about 2 ℃/min.
In view of further improving the aging resistance of the material, the composite film has a breaking strength retention rate of more than 50% and a peel strength of more than 1N/cm after being subjected to an oil aging test for 8 times of circulation. The breaking strength retention is preferably more than 60%. Considering that the material needs to maintain toughness to some extent, the composite film is further preferably subjected to an oil aging test of 8 cycles, and the composite film has an elongation at break retention rate of more than 30% and a dielectric breakdown voltage of more than 8 kV.
In addition to oil aging performance, sometimes, the composite film is required to have a certain degree of wet heat aging performance to meet the actual use requirements. Furthermore, after the composite film is subjected to a damp-heat aging test, the breaking strength retention rate is more than 80%, the breaking elongation retention rate is more than 70%, the peel strength is more than 1N/cm, and the dielectric breakdown voltage is more than 8 kV. The humid heat aging test refers to an aging test in which a sample is left at 120 ℃ and 100% RH for 240 hours. If the composite film does not achieve the above properties after the damp heat aging test, the composite film may have too low strength, too high brittleness, or a risk of degumming, or too poor insulation properties, and the possibility of material failure during actual use may exist.
The polymer film layer may be any polymer film that provides the composite film with the above-described properties. Preferably, the film is one or more of a polyester film such as PET or PEN, a PPS film, a polyether ether ketone (PEEK) film, an aromatic polyamide (aromatic PA) film, or a PI film. The term "PET, PEN, PPS, PEEK, aromatic PA, or PI film" means that one or more additives such as a lubricant, a colorant, and a crystallization nucleating agent, or other polymers may be mixed in the film, or a copolymer of PET, PEN, PPS, PEEK, aromatic PA, or PI may be used.
In view of providing a composite film excellent in aging resistance, chemical resistance, mechanical characteristics and/or processability, it is preferable that at least one of the polymer film layers is a PPS film layer.
The PPS film component preferably contains 60 mass% or more of a PPS resin. When the content of the PPS resin is less than 60 mass%, crystallinity, glass transition temperature, and the like of the composition become low, and aging resistance, thermal dimensional stability, mechanical properties, and the like of a film including the composition are lowered. The PPS resin is preferably a polymer containing 80 mol% or more of PPS units. When the PPS unit is less than 80 mol%, the crystallinity of the polymer is insufficient, and the aging resistance, thermal dimensional stability, mechanical characteristics, and the like of the film comprising the polymer are impaired.
In view of further improving the durability of the composite film, it is further preferable that at least one of the polymer film layers is a biaxially stretched PPS film layer.
The PPS film layer can be produced by melt molding a resin composition containing PPS as a main component. If the film is then biaxially stretched, a biaxially stretched PPS film layer can be obtained. For example, the PPS film layer may be one obtained from Tolli corporation
The PPS film may be a single layer, or may be a multilayer film obtained by laminating 2 or more layers of single-layer PPS films.
The composite film preferably comprises an aramid paper layer. Examples of the aramid, i.e., aromatic polyamide, include polyisophthaloyl metaphenylene diamine or a copolymer thereof, polyparaphenylene terephthalamide or a copolymer thereof, and copoly (p-phenylene-3, 4' -diphenylether terephthalamide). The method or source for preparing the aramid paper is not particularly limited in the present invention. Aramid paper can generally be prepared by the following method: for example, the aramid and the aramid are mixed at a weight ratio of 5/95 to 95/5, preferably 10/90 to 90/10, and then formed into a sheet. Specifically, for example: a method of forming a sheet by a gas flow after dry-mixing the aramid and the aramid, a method of dispersing and mixing the aramid and the aramid in a liquid medium, discharging the mixture onto a liquid-permeable support, forming a sheet, removing the liquid, and drying the sheet, and the like. The aramid paper obtained as described above is hot-pressed between a pair of rolls at high temperature and high pressure, whereby the density and mechanical strength can be improved. Multiple sheets of aramid paper may also be laminated during hot pressing. The hot press working may be performed a plurality of times in any order. The aramid paper layer may also be selected from Nomex available from DuPont.
Further, in view of improving the peel strength of the material, it is preferable to surface-treat the surface of the film layer and/or the aramid paper layer to improve the adhesion thereof to the adhesive layer. The surface treatment may be a corona treatment, a flame treatment, a plasma treatment, an acid treatment, or the like. The composite film is provided with an adhesive layer. The adhesive layer comprises at least one adhesive selected from the group consisting of: phenolic resins, urea-formaldehyde resins, polyvinyl acetates, epoxies, polyurethanes, silicones, unsaturated polyesters, acrylics, proteins, carbohydrates, or synthetic rubber adhesives.
In view of aging resistance, insulation and/or environmental protection, one or more of epoxy-based, polyurethane-based, acrylic-based, or silicone-based adhesives are preferable. The type of the adhesive is not particularly required, and can be reactive or non-reactive; can be thermally cured, moisture cured, photo cured, or can be cured in a variety of ways. Can be a single-component type or a two-component type. Further, in view of improving oil resistance and hydrolysis resistance, a polyester urethane adhesive, an acrylic modified polyester urethane adhesive, or a one-component silicone adhesive is preferable. The method for forming the adhesive layer is not particularly limited, and examples thereof include a method of coating and drying an adhesive solution on a film, a method of transferring by a release sheet provided with an adhesive layer, and the like. The coating method may be a roll coating method such as reverse coating or gravure coating, a spin coating method, a screen coating method, a spray coating method, a dip coating method, a spray coating method, or the like. Then, a proper composite film preparation method can be selected by combining with the actual conditions such as the formation method of the adhesive layer and the like, such as a composite method of dry compounding, wet compounding, extrusion compounding, coextrusion compounding, solvent-free compounding, hot melt adhesive compounding and the like, or the comprehensive use of various composite methods. The increased thickness can improve the aging resistance, rigidity and other properties of the material, but at the same time, the flexibility is reduced, and the increased weight of the product is not favorable for the light weight and high performance of the engine. Therefore, it is necessary to reduce the thickness of the composite film as much as possible on the premise that the performance meets the actual use requirements. The overall thickness of the composite film is preferably 50 to 500. mu.m, more preferably 80 to 300. mu.m, depending on the practical application. The thickness of each single polymer film layer and each aramid paper layer which form the composite film is preferably 10-200 mu m. The thickness of the single-layer adhesive layer is preferably about 5-40 μm.
The number of layers is not particularly limited, and preferably 4 to 8 layers. The preferred layer structure is aramid paper/adhesive/PPS film/adhesive/aramid paper. In view of providing better durability, it is further preferable that the total thickness of the aramid paper is smaller than that of the PPS film. The aramid paper on the two sides of the PPS film can be consistent or inconsistent in thickness, and technical personnel can carry out reasonable arrangement according to actual requirements.
Considering that the composite film needs to have certain rigidity, peeling strength and insulating property, it is further preferable that the breaking strength of the composite film is more than 120MPa, the peeling strength is more than 2N/cm, and the dielectric breakdown voltage is more than 10 kV.
Considering that the composite film needs to have certain oil resistance, the composite film is further preferably subjected to an oil aging test of 8 times of circulation, and has a breaking strength of more than 80MPa and an elongation at break of more than 10%.
The composite film can be used as an insulating film and used in various occasions needing electric insulation, including new energy automobile motors. And can be used for industrial and civil applications such as packaging materials, structural materials, building materials and decorative materials.
Detailed Description
The present invention is described in more detail by the following examples, which are not intended to limit the present invention.
The aging test method used in the examples and comparative examples is as follows:
humid heat aging test:
after the sample was left at 120 ℃ and 100% RH for 240 hours, the sample was taken out and tested for various properties.
Oil aging test:
the sample was immersed in a mixed liquid consisting of 99.5 vol% of automatic transmission oil (DEXRON VI, Petro Canada) and 0.5 vol% of water, warmed from room temperature to 155 ℃ at a rate of about 2 ℃/min for 40 hours, then cooled to-45 ℃ at a rate of about 2 ℃/min for 8 hours, and then warmed to room temperature at a rate of about 2 ℃/min for one cycle. After 4 or 8 cycles, samples were removed and tested for various properties.
The test methods used in the examples and comparative examples are as follows:
thickness: the total thickness of the test specimens was determined by a Sanyo Instrument model 7050 thickness gauge, and the 9 data were averaged.
Breaking strength and retention rate thereof, elongation at break and retention rate thereof: the test piece was produced by a DUMBBELL SD-100 test piece producing machine, and cut out in the MD direction of the sample to have a width of 10mm, a length of 150mm, and an actual tensile length of 100 mm. Then, the breaking strength and the breaking elongation of the specimen were measured by a tensile tester AG-IS 1KN manufactured by Shimadzu corporation, Japan. The drawing speed was 200 mm/min. The number of test repetitions was 5, taking the maximum of 3 values. The retention was calculated as in formula 1 and formula 2:
breaking strength retention rate ═ breaking strength after aging test/breaking strength before aging test × 100% (formula 1); the retention rate of elongation at break is the elongation at break after the aging test/the elongation at break before the aging test × 100% (formula 2).
Peel strength: the test piece was produced by a DUMBBELL SD-100 test piece producing machine, and was sampled in the MD direction of the sample with a width of 10mm and a length of 150 mm. Then, the interlaminar 180 ℃ peel strength of the sample was measured by a tensile tester AG-IS 1KN manufactured by Shimadzu corporation. The peeling rate speed was 200 mm/min. The number of test repetitions was 5, taking the maximum of 3 values. The 180-degree interlayer peel strength refers to the peel strength between the film layer and the non-adhesive layer closest to the film layer, and when a certain sample has a plurality of 180-degree interlayer peel strengths, the minimum value is taken as the peel strength of the sample.
Dielectric breakdown voltage: the voltage was measured by an AC withstand voltage tester manufactured by ウェッジ Japan in an AC mode with an electrode diameter of 25mm and a voltage increasing speed of 1.0 kV/s. The sample size was 120mm x 120mm, the number of test repetitions was 5, and the average was taken.
The raw materials used in the examples:
aramid paper a: manufactured by DuPont, model Nomex T464, 50 μm thick.
Aramid paper B: manufactured by DuPont, model Nomex T464, with a thickness of 80 μm.
Aramid paper C: manufactured by DuPont, model Nomex T410, 50 μm thick.
PPS film A: biaxially oriented PPS film manufactured by dongli corporation, model: 3F40, thickness 115 μm.
PPS film B: a PPS film produced by Toray corporation, which was not biaxially stretched, had a thickness of 125 μm.
Adhesive A: the adhesive is a single-component polyester type moisture-curing polyurethane adhesive which is produced by Zhejiang Taiwan adhesive Material Ming, Midebang, and has the model M2501, the solid content of 50 percent and the solvent of ethyl acetate.
And (3) adhesive B: the adhesive is a bi-component thermosetting polyurethane adhesive which is produced by Shanghai Toyo ink manufacturing company Limited and has the model TM-K76-CN/CAT-10-CN, the solid contents are respectively 51 percent and 75 percent, and the solvent is ethyl acetate. Before use, the mixture was mixed with TM-K76-CN/CAT-10-CN 15/1 (weight ratio).
Adhesive C: the type K5906T of Guangdong Hengda New Material science and technology Limited company, and the one-component organic silicon adhesive.
And (3) adhesive D: the adhesive is prepared from a bi-component thermosetting polyester polyurethane adhesive which is produced by Shanghai Toyo ink manufacturing company Limited and has the model TM-K55-CN/CAT-10-CN, the solid contents of which are respectively 30 percent and 75 percent, and the solvent is ethyl acetate. Before use, the mixture was mixed with TM-K55-CN/CAT-10-CN 7/1 (weight ratio).
And (3) adhesive E: the adhesive is a bi-component thermosetting acrylic polyurethane adhesive, wherein the adhesive is produced by Midebang adhesive materials Limited, Taiwan, Zhejiang, and is in a model D902M-A/D902M-B, the solid contents are 34% and 75% respectively, and the solvent is butyl acetate. The mixture was blended at D902M-A/D902M-B3/1 (weight ratio) before use.
Example 1
Coating an adhesive E with a certain thickness on one surface of a PPS film A, drying at 130 ℃, compounding aramid fiber paper A on the surface by using a film coating machine, compounding at the temperature of 100 ℃, then coating an adhesive E with a certain thickness on the other surface of the PPS film A, drying at 130 ℃, compounding another layer of aramid fiber paper A on the surface by using a film coating machine, compounding at the temperature of 100 ℃, and then placing at 80 ℃ for 3 days to obtain the composite film with a 5-layer structure of aramid fiber paper/adhesive/PPS film/adhesive/aramid fiber paper, wherein the thickness of a single-layer adhesive is 10 mu m. The results of the tests carried out after 2 days at room temperature are shown in Table 1.
Example 2
Coating an adhesive A with a certain thickness on one surface of a PPS film A, drying at 80 ℃, compounding aramid fiber paper A on the surface by using a film coating machine at the compounding temperature of 100 ℃, then coating the adhesive A with a certain thickness on the other surface of the PPS film A, drying at 80 ℃, compounding another layer of aramid fiber paper A on the surface by using a film coating machine at the compounding temperature of 100 ℃, and obtaining the composite film with a 5-layer structure of aramid fiber paper/adhesive/PPS film/adhesive/aramid fiber paper, wherein the thickness of the single-layer adhesive is 10 mu m. The test pieces were then allowed to stand at room temperature for 2 days, and the results are shown in Table 1.
Example 3
Coating an adhesive A with a certain thickness on one surface of a PPS film B, drying at 80 ℃, compounding aramid fiber paper A on the surface by using a film coating machine at the compounding temperature of 100 ℃, then coating the adhesive A with a certain thickness on the other surface of the PPS film B, drying at 80 ℃, compounding another layer of aramid fiber paper A on the surface by using a film coating machine at the compounding temperature of 100 ℃, and obtaining the composite film with a 5-layer structure of aramid fiber paper/adhesive/PPS film/adhesive/aramid fiber paper, wherein the thickness of the single-layer adhesive is 10 mu m. The test pieces were then allowed to stand at room temperature for 2 days, and the results are shown in Table 1.
Example 4
Coating an adhesive B with a certain thickness on one surface of a PPS film A, drying at 80 ℃, compounding aramid fiber paper A on the surface by using a film coating machine, compounding at the temperature of 40 ℃, then coating an adhesive B with a certain thickness on the other surface of the PPS film A, drying at 80 ℃, compounding another layer of aramid fiber paper A on the surface by using a film coating machine, compounding at the temperature of 40 ℃, and then placing at 60 ℃ for 3 days to obtain the composite film with a 5-layer structure of aramid fiber paper/adhesive/PPS film/adhesive/aramid fiber paper, wherein the thickness of a single-layer adhesive is 10 mu m. The composite film was subjected to various tests, and the results are shown in table 1.
Example 5
Coating an adhesive C with a certain thickness on one surface of a PPS film A, compounding aramid fiber paper A on the surface by using a film laminating machine at the compounding temperature of 40 ℃, then coating the adhesive C with a certain thickness on the other surface of the PPS film A, compounding another layer of aramid fiber paper A on the surface by using a film laminating machine at the compounding temperature of 40 ℃, and standing for 1 day at room temperature and 50% RH to obtain the composite film with the structure of 5 layers of aramid fiber paper/adhesive/PPS film/adhesive/aramid fiber paper, wherein the thickness of the single-layer adhesive is 10 mu m. The composite film was subjected to various tests, and the results are shown in table 1.
Example 6
Coating an adhesive D with a certain thickness on one surface of a PPS film A, drying at 80 ℃, compounding aramid fiber paper A on the surface by using a film coating machine, compounding at the temperature of 40 ℃, then coating an adhesive D with a certain thickness on the other surface of the PPS film A, drying at 80 ℃, compounding another layer of aramid fiber paper A on the surface by using a film coating machine, compounding at the temperature of 40 ℃, and then placing at 60 ℃ for 3 days to obtain the composite film with a 5-layer structure of aramid fiber paper/adhesive/PPS film/adhesive/aramid fiber paper, wherein the thickness of a single-layer adhesive is 10 mu m. The composite film was subjected to various tests, and the results are shown in table 1.
Example 7
Coating an adhesive E with a certain thickness on one surface of a PPS film A, drying at 130 ℃, compounding aramid fiber paper B on the surface by using a film coating machine, compounding at the temperature of 100 ℃, then coating an adhesive E with a certain thickness on the other surface of the PPS film A, drying at 130 ℃, compounding another layer of aramid fiber paper B on the surface by using a film coating machine, compounding at the temperature of 100 ℃, and then placing at 80 ℃ for 3 days to obtain the composite film with a 5-layer structure of aramid fiber paper/adhesive/PPS film/adhesive/aramid fiber paper, wherein the thickness of a single-layer adhesive is 10 mu m. The results of the tests carried out after 2 days at room temperature are shown in Table 1.
Example 8
Coating an adhesive E with a certain thickness on one surface of a PPS film A, drying at 130 ℃, compounding aramid fiber paper C on the surface by using a film coating machine, compounding at the temperature of 100 ℃, then coating an adhesive E with a certain thickness on the other surface of the PPS film A, drying at 130 ℃, compounding another layer of aramid fiber paper C on the surface by using a film coating machine, compounding at the temperature of 100 ℃, and then placing at 80 ℃ for 3 days to obtain the composite film with a 5-layer structure of aramid fiber paper/adhesive/PPS film/adhesive/aramid fiber paper, wherein the thickness of a single-layer adhesive is 10 mu m. The results of the tests carried out after 2 days at room temperature are shown in Table 1.
Comparative example 1
Aramid paper, model Nomex T410 from dupont, 250 μm thick. The paper was subjected to the tests and the results are shown in table 2. Since the paper was not a composite film, the peel strength was not tested. Since it is difficult to completely remove the oil absorbed in the paper, the dielectric breakdown voltage of the sample subjected to the oil aging test is slightly increased by the presence of the oil inside the paper.
Comparative example 2
Aramid paper/PPS film/aramid paper 3-layer structured composite film (NSN), model Namli NSN343A, available from wamura industries, having a thickness of 240 μm. The composite film is formed by hot pressing a single-layer material subjected to low-temperature plasma surface treatment without using an adhesive. The composite film was subjected to various tests, and the results are shown in Table 2. After an oil aging test, various performances are reduced, and particularly the peeling strength is obviously reduced.
Comparative example 3
Aramid paper/PET film/aramid paper composite film (NMN) purchased from Schchangcheng island insulation materials Co., Ltd, model number NMN 250T, and having a thickness of 250 μm.
The composite film was subjected to various tests, and the results are shown in Table 2. However, the aramid paper and the PET layer of the composite film were delaminated after the wet heat aging test, so the peel strength was not tested. After the composite film is subjected to oil aging tests for 4 times, the PET layer is damaged, the service performance is lost, and various performances cannot be tested.
Comparative example 4
Aramid paper/PI film/aramid paper composite film (NHN) available from Schchangcheng insulant Co., Ltd, model NHN 250T, thickness 250 μm.
The composite film was subjected to various tests, and the results are shown in Table 2. However, the aramid paper and the PI layer of the composite film were delaminated after the wet heat aging test, so the peel strength was not tested. After the composite film is subjected to oil aging tests for 4 times, the PI layer is damaged, the use performance is lost, and various performances cannot be tested.
Further, the processability of each sample of examples 1 to 8 and comparative examples 1 to 4 was actually measured using an automatic insulation film inserting machine. As a result, examples 1 to 8 and comparative examples 3 to 4 all had better processability. Comparative example 1 had poor rigidity, insertion was difficult, and processability was poor. Comparative example 2 was easily delaminated during processing and had poor processability.
Compared with Nomex in comparative example 1, the multilayer composite film has higher rigidity, insulativity and aging resistance; compared with the NSN of the comparative example 2, the NSN has the advantages of difficult fracture during processing and good processability, and simultaneously shows better aging resistance; the aging resistance was better than that of the NMN and NHN described in comparative examples 3 and 4.
TABLE 1
TABLE 1 (continuation)
Samples with peel strength >3N/cm, where cohesive failure of the surface layer of the sample occurred during the peel test, the peel strength at this time was read as about 3N/cm, but actually the peel strength was greater than this. So it is recorded as > 3N/cm.
The interlaminar peeling indicates that the surface layer and the inner layer of the sample are separated due to the damage of the adhesive layer.
TABLE 2
Material failure means that the inner layer of the sample was broken, so various tests could not be performed.
Claims (9)
1. A composite film characterized by: the composite film is provided with one or more polymer film layers and one or more adhesive layers, after the composite film is subjected to an oil aging test for 4 times, the breaking strength retention rate is more than 50%, the breaking elongation retention rate is more than 53%, the peel strength is more than 1N/cm, at least one of the polymer film layers is a polyphenylene sulfide film layer, and the composite film contains an aramid paper layer.
2. The composite film of claim 1, wherein: after the composite film is subjected to an oil aging test for 4 times, the breaking elongation retention rate is more than 30%, and the insulation breakdown voltage is more than 8 kV.
3. The composite film of claim 1, wherein: after the composite film is subjected to an oil aging test for 8 times, the fracture strength retention rate is more than 50%, and the peel strength is more than 1N/cm.
4. The composite film of claim 2, wherein: after the composite film is subjected to an oil aging test for 8 times, the breaking elongation retention rate is more than 30%, and the insulation breakdown voltage is more than 8 kV.
5. The composite film of claim 1, wherein: after the composite film is subjected to a damp-heat aging experiment, the breaking strength retention rate is more than 80%, the breaking elongation retention rate is more than 70%, the peeling strength is more than 1N/cm, and the dielectric breakdown voltage is more than 8 kV.
6. The composite film of claim 1, wherein: at least one layer of the polymer film layers is a two-way stretching polyphenylene sulfide film layer.
7. The composite film of claim 1, wherein: the adhesive is one or more of epoxy, polyurethane, acrylic or organosilicon adhesives.
8. The composite film of claim 1, wherein: the breaking strength of the composite film is more than 120MPa, the peeling strength is more than 2N/cm, and the dielectric breakdown voltage is more than 10 kV.
9. The composite film of claim 1, wherein: after the composite film is subjected to an oil aging test for 8 times, the breaking strength is greater than 80MPa, and the breaking elongation is greater than 10%.
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| CN111477876A (en) * | 2019-01-24 | 2020-07-31 | 东丽先端材料研究开发（中国）有限公司 | Multilayer film, current collector, pole piece and battery |
| CN110031302A (en) * | 2019-04-19 | 2019-07-19 | 国网四川省电力公司电力科学研究院 | A kind of capacitor BOPP film ageing properties test method |
| CN112172270A (en) * | 2019-07-05 | 2021-01-05 | 东丽先端材料研究开发（中国）有限公司 | Composite film |
| CN112238664B (en) * | 2019-07-18 | 2024-05-03 | 东丽先端材料研究开发（中国）有限公司 | Film material for thermosetting resin molding and molded product thereof |
| CN112358637B (en) * | 2020-11-03 | 2022-06-21 | 浙江新和成特种材料有限公司 | Polyphenylene sulfide film suitable for ultrathin coating and preparation method and application thereof |
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| DE102004002385A1 (en) * | 2004-01-15 | 2005-08-11 | Weiss Kunststofftechnik Gmbh | Composite film and plastic product manufacture involves molding plastic directly onto formed plastic film in tool where bond is created without use of additional adhesive |
| CN101877259A (en) * | 2009-12-25 | 2010-11-03 | 四川东材绝缘技术有限公司 | High temperature resistant electrical soft composite material and manufacturing method thereof |
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|---|---|---|---|---|
| DE102004002385A1 (en) * | 2004-01-15 | 2005-08-11 | Weiss Kunststofftechnik Gmbh | Composite film and plastic product manufacture involves molding plastic directly onto formed plastic film in tool where bond is created without use of additional adhesive |
| CN101877259A (en) * | 2009-12-25 | 2010-11-03 | 四川东材绝缘技术有限公司 | High temperature resistant electrical soft composite material and manufacturing method thereof |
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