CN117106217B - Corona-resistant polyimide-poly (perfluoroethylene-propylene) composite film and preparation method thereof - Google Patents
Corona-resistant polyimide-poly (perfluoroethylene-propylene) composite film and preparation method thereof Download PDFInfo
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- CN117106217B CN117106217B CN202311028306.3A CN202311028306A CN117106217B CN 117106217 B CN117106217 B CN 117106217B CN 202311028306 A CN202311028306 A CN 202311028306A CN 117106217 B CN117106217 B CN 117106217B
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- propylene
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- perfluoroethylene
- corona
- polyimide
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- 239000002131 composite material Substances 0.000 title claims abstract description 92
- 238000002360 preparation method Methods 0.000 title abstract description 75
- -1 poly (perfluoroethylene-propylene) Polymers 0.000 claims abstract description 59
- 239000007788 liquid Substances 0.000 claims abstract description 53
- XIUFWXXRTPHHDQ-UHFFFAOYSA-N prop-1-ene;1,1,2,2-tetrafluoroethene Chemical group CC=C.FC(F)=C(F)F XIUFWXXRTPHHDQ-UHFFFAOYSA-N 0.000 claims abstract description 43
- 229920001721 polyimide Polymers 0.000 claims abstract description 38
- 239000006185 dispersion Substances 0.000 claims abstract description 25
- 238000001035 drying Methods 0.000 claims abstract description 23
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 21
- 239000000463 material Substances 0.000 claims abstract description 15
- 229920006322 acrylamide copolymer Polymers 0.000 claims abstract description 13
- 239000011248 coating agent Substances 0.000 claims abstract description 13
- 238000000576 coating method Methods 0.000 claims abstract description 13
- 239000000945 filler Substances 0.000 claims abstract description 13
- VGPXMTPKYDNMQA-UHFFFAOYSA-N furan-2,5-dione;prop-2-enamide Chemical compound NC(=O)C=C.O=C1OC(=O)C=C1 VGPXMTPKYDNMQA-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 10
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 41
- 229910052582 BN Inorganic materials 0.000 claims description 26
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 claims description 17
- 239000004094 surface-active agent Substances 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 14
- NBVXSUQYWXRMNV-UHFFFAOYSA-N fluoromethane Chemical compound FC NBVXSUQYWXRMNV-UHFFFAOYSA-N 0.000 claims description 12
- VOZRXNHHFUQHIL-UHFFFAOYSA-N glycidyl methacrylate Chemical compound CC(=C)C(=O)OCC1CO1 VOZRXNHHFUQHIL-UHFFFAOYSA-N 0.000 claims description 10
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 9
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 claims description 9
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 8
- 239000011734 sodium Substances 0.000 claims description 8
- 229910052708 sodium Inorganic materials 0.000 claims description 8
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 6
- 238000011049 filling Methods 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims 1
- 230000000052 comparative effect Effects 0.000 description 19
- 239000000243 solution Substances 0.000 description 18
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 10
- 230000004048 modification Effects 0.000 description 6
- 238000012986 modification Methods 0.000 description 6
- 238000009413 insulation Methods 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 239000011159 matrix material Substances 0.000 description 4
- 238000011056 performance test Methods 0.000 description 4
- 238000010998 test method Methods 0.000 description 4
- 239000004642 Polyimide Substances 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 230000001681 protective effect Effects 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 239000004812 Fluorinated ethylene propylene Substances 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 239000012752 auxiliary agent Substances 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- HQQADJVZYDDRJT-UHFFFAOYSA-N ethene;prop-1-ene Chemical group C=C.CC=C HQQADJVZYDDRJT-UHFFFAOYSA-N 0.000 description 2
- 230000007774 longterm Effects 0.000 description 2
- 239000003607 modifier Substances 0.000 description 2
- 238000007719 peel strength test Methods 0.000 description 2
- 229920009441 perflouroethylene propylene Polymers 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 239000012744 reinforcing agent Substances 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 2
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 239000002612 dispersion medium Substances 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- FCZCIXQGZOUIDN-UHFFFAOYSA-N ethyl 2-diethoxyphosphinothioyloxyacetate Chemical compound CCOC(=O)COP(=S)(OCC)OCC FCZCIXQGZOUIDN-UHFFFAOYSA-N 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/04—Coating
- C08J7/0427—Coating with only one layer of a composition containing a polymer binder
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D127/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers
- C09D127/02—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment
- C09D127/12—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
- C09D127/18—Homopolymers or copolymers of tetrafluoroethene
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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
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/47—Levelling agents
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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
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
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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
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
- C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
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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
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/65—Additives macromolecular
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/70—Additives characterised by shape, e.g. fibres, flakes or microspheres
-
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2379/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen, or carbon only, not provided for in groups C08J2361/00 - C08J2377/00
- C08J2379/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
- C08J2379/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
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- C08J2427/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers
- C08J2427/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
- C08J2427/12—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
- C08J2427/18—Homopolymers or copolymers of tetrafluoroethylene
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/38—Boron-containing compounds
- C08K2003/382—Boron-containing compounds and nitrogen
- C08K2003/385—Binary compounds of nitrogen with boron
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- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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Abstract
The application relates to the field of corona-resistant materials, and discloses a corona-resistant polyimide-poly perfluoroethylene propylene composite film and a preparation method thereof, wherein the corona-resistant polyimide-poly perfluoroethylene propylene composite film consists of a polyimide film layer and a poly perfluoroethylene propylene layer, the poly perfluoroethylene propylene layer is prepared by solidifying a poly perfluoroethylene propylene composite liquid, and the poly perfluoroethylene propylene composite liquid is prepared from the following raw materials in parts by weight: 60-80 parts of a perfluoroethylene propylene dispersion liquid, 8-20 parts of a filler, 3-8 parts of a leveling agent and 5-15 parts of a maleic anhydride-acrylamide copolymer; the preparation method comprises the following steps: and (3) coating the poly (perfluoroethylene-propylene) composite liquid on the surface of the polyimide film layer, and drying to obtain the polyimide film. The preparation method is simple, the prepared perfluoroethylene propylene layer and the polyimide film layer are stable in adhesion and not easy to separate, and the prepared corona-resistant polyimide-poly perfluoroethylene propylene composite film has good stability, flexibility and corona resistance.
Description
Technical Field
The application relates to the field of corona-resistant materials, in particular to a corona-resistant polyimide-poly (perfluoroethylene-propylene) composite film and a preparation method thereof.
Background
The surface and the belt layer of the insulating protective material for the high-voltage power cable, the joint and the terminal of the high-voltage power cable can lead to the phenomenon that gas is partially dissociated to generate discharge under the action of a strong electric field, namely corona, the dissociated ions and electrons impact a high polymer chain, and the action of ozone generated by discharge and the local heating phenomenon can lead the insulating protective material to generate cracking to cause embrittlement and cracking, so that the capability of the edge protective material for resisting the corona to keep a use function is called corona resistance.
Polyimide film has excellent performances such as high heat resistance, strong insulation and radiation resistance, so that the polyimide film is widely applied to insulation protection materials of various high temperature resistant motors, electric appliances and cables, in order to improve corona resistance of the insulation protection materials, the single-sided or double-sided of the polyimide film is coated with the poly (perfluoroethylene propylene) to form the poly (perfluoroethylene propylene) -polyimide composite film with the poly (perfluoroethylene propylene) layer, but in the long-term use process, the poly (perfluoroethylene propylene) layer of the poly (perfluoroethylene propylene) -polyimide composite film is easy to separate from the polyimide film, so that the corona resistance is affected.
Disclosure of Invention
In order to solve the problem that a poly (perfluoroethylene propylene) layer of a poly (perfluoroethylene propylene) -polyimide composite film which is conventionally used is easy to separate and the corona resistance is reduced, the application provides a corona resistant polyimide-poly (perfluoroethylene propylene) composite film and a preparation method thereof.
In a first aspect, the present application provides a corona resistant polyimide-poly perfluoroethylene propylene composite film, which adopts the following technical scheme:
the corona-resistant polyimide-poly perfluoroethylene propylene composite film consists of a polyimide film layer and a poly perfluoroethylene propylene layer arranged on the surface of the polyimide film layer, wherein the poly perfluoroethylene propylene layer is prepared by solidifying poly perfluoroethylene propylene composite liquid, and the poly perfluoroethylene propylene composite liquid is prepared from the following raw materials in parts by weight:
60-80 parts of a dispersion of perfluoroethylene propylene
8-20 parts of filling material
3-8 parts of leveling agent
5-15 parts of maleic anhydride-acrylamide copolymer.
By adopting the technical scheme, the poly (perfluoroethylene propylene) dispersion liquid is used as a dispersion matrix, the filler is added into the matrix to serve as a performance reinforcing agent, the effect of improving the mechanical property and heat resistance of the prepared poly (perfluoroethylene propylene) layer is achieved, the addition of the leveling agent can better improve the coating stability of the prepared poly (perfluoroethylene propylene) composite liquid on the surface of the polyimide film layer, further the adhesive force of the poly (perfluoroethylene propylene) layer is improved, the maleic anhydride-acrylamide copolymer is a polymer with better compatibility and dispersibility, better synergistic effect can be produced with the leveling agent, the dispersion uniformity of the filler in the poly (perfluoroethylene propylene) dispersion liquid is improved, the condition that the system is unstable due to the addition of the leveling agent and the filler is reduced, meanwhile, the maleic anhydride-acrylamide copolymer and the polyimide film have relatively similar molecular polarity, the adhesive stability of the prepared poly (perfluoroethylene propylene) composite liquid can be improved, and further the prepared poly (perfluoroethylene propylene) layer is not easy to be separated from the polyimide film layer, and the polyimide film with good mechanical property and good heat resistance and heat resistance.
Preferably, the filling material consists of spherical alumina and boron nitride with the dosage ratio of 1 (0.4-0.6).
By adopting the technical scheme, the spherical alumina has relatively low cost and good heat resistance, the boron nitride has good heat resistance, insulation and mechanical properties, and the spherical alumina and the boron nitride with better proportion are used as the filling materials in the technical scheme of the application, so that the prepared poly-perfluoroethylene propylene layer has reasonable cost and good heat resistance, heat conductivity and mechanical properties.
Preferably, the boron nitride is modified boron nitride, and the modified boron nitride is prepared from the following raw materials in parts by weight:
silane coupling agent KH-792-5 parts
1-3 parts of sodium isobenzenesulfonate
80-120 parts of 50-80wt% ethanol water solution
50-70 parts of boron nitride.
By adopting the technical scheme, the modified boron nitride with uniform dispersion performance and good compatibility in the perfluoroethylene propylene dispersion liquid is prepared by taking the ethanol water solution with better concentration as the dispersion medium of the boron nitride, taking the silane coupling agent KH-792 as the modifier and taking sodium isobenzene sulfonate as the modification auxiliary agent.
Preferably, the modified boron nitride is prepared by the steps of:
adding boron nitride into 50-80wt% ethanol water solution, stirring uniformly, heating to 60-70 ℃, adding sodium isobenzenesulfonate and silane coupling agent KH-792 for reaction for 1-2h, cooling, suction filtering, drying, crushing and grinding to obtain modified boron nitride.
According to the technical scheme, firstly, boron nitride is dispersed in an ethanol aqueous solution, then the silane coupling agent KH-792 is used for carrying out surface modification on the boron nitride, the dispersion uniformity of the boron nitride in the perfluoroethylene propylene dispersion liquid is improved, sodium isobenzenesulfonate is added in the modification, the hydrophilicity of the boron nitride can be further improved, the grafting effect of the boron nitride and the silane coupling agent KH-792 is further improved, the modification efficiency of the boron nitride is improved, the modified boron nitride is added into the perfluoroethylene propylene dispersion liquid, the boron nitride can be uniformly dispersed and is not easy to agglomerate, the prepared perfluoroethylene propylene composite liquid system is uniform and stable, the surface of a polyimide film layer can be uniformly dispersed and coated, the mechanical property, the adhesion property and the heat conduction heat resistance of the prepared corona resistant polyimide-perfluoroethylene propylene composite film are improved, and the corona resistance is further improved.
Preferably, the leveling agent consists of glycidyl methacrylate and fluorocarbon surfactant in the dosage ratio of (0.3-0.5): 1.
By adopting the technical scheme, the glycidyl methacrylate has better bonding performance, can be stably dispersed in the perfluoroethylene propylene dispersion liquid, and the fluorocarbon surfactant has better dispersibility and wettability, so that the surface tension of the prepared perfluoroethylene propylene composite liquid can be reduced, the glycidyl methacrylate and the fluorocarbon surfactant with better proportion are used as flatting agents, the prepared perfluoroethylene propylene composite liquid has better wetting and bonding capabilities on a polyimide film layer, can be stably attached to the surface of the polyimide film layer, and improves the stability and corona resistance of the prepared corona-resistant polyimide-perfluoroethylene propylene composite film.
Preferably, the polyperfluoroethylene propylene composite liquid is prepared by the following steps: adding the perfluoroethylene propylene dispersion liquid, the flatting agent, the maleic anhydride-acrylamide copolymer and the filler into stirring equipment, and uniformly stirring to obtain the perfluoroethylene propylene composite liquid.
By adopting the technical scheme, the polyperfluoroethylene propylene composite liquid with stable system and uniform dispersion is prepared.
Preferably, the mixing and stirring time is 1-3h, and the stirring speed is 800-1200rpm.
By adopting the technical scheme, the prepared fluorinated ethylene propylene composite liquid system can be uniformly dispersed due to the better mixing and stirring speed and stirring time.
Preferably, the thickness of the fluorinated ethylene propylene layer is 20-50 μm.
By adopting the technical scheme, the corona-resistant polyimide-poly perfluoroethylene propylene composite film prepared by the poly perfluoroethylene propylene layer with the better thickness has better corona resistance.
In a second aspect, the present application provides a method for preparing a corona resistant polyimide-poly perfluoroethylene propylene composite film, which adopts the following technical scheme:
the preparation method of the corona-resistant polyimide-poly (perfluoroethylene-propylene) composite film comprises the following preparation steps:
and coating the poly (perfluoroethylene-propylene) composite liquid on the surface of the polyimide film layer to form a poly (perfluoroethylene-propylene) layer, and drying to obtain the corona-resistant polyimide-poly (perfluoroethylene-propylene) composite film.
By adopting the technical scheme, the corona-resistant polyimide-poly perfluoroethylene propylene composite film is uniformly attached to the surface of the polyimide film layer in a coating mode, and the corona-resistant polyimide-poly perfluoroethylene propylene composite film with stable performance is prepared by drying.
Preferably, the coating rate of the poly (perfluoroethylene-propylene) composite solution is 1.5-2.5m/min, and the drying is divided into two stages, wherein the drying temperature in the first stage is 260-280 ℃, the drying time is 6-8min, the drying temperature in the second stage is 310-330 ℃, and the drying time is 1-3min.
Through adopting above-mentioned technical scheme, the even coating in polyimide film layer's surface of the compound liquid of the perfluoro ethylene propylene of better coating rate can be made, and the better drying temperature can make the compound liquid of the perfluoro ethylene propylene form even closely knit perfluoro ethylene propylene layer of the perfluoro ethylene propylene of the perfluoro, promotes the adhesiveness of the perfluoro ethylene propylene layer of the perfluoro ethylene, makes the stable complex of perfluoro ethylene propylene layer and the perfluoro ethylene propylene layer of the perfluoro ethylene, and difficult separation promotes the corona resistance performance of the corona resistant polyimide-perfluoro ethylene propylene composite film of making.
In summary, the present application has the following beneficial effects:
1. according to the corona-resistant polyimide-poly perfluoroethylene propylene composite film, the poly perfluoroethylene propylene dispersion liquid is used as a matrix, the filler is added into the matrix to serve as a performance reinforcing agent, the leveling agent and the maleic anhydride-acrylamide copolymer are added, under the synergistic effect of the two, the dispersion uniformity stability of the prepared poly perfluoroethylene propylene composite liquid and the adhesiveness of the prepared poly perfluoroethylene propylene composite film with a polyimide film layer are improved, and the prepared corona-resistant polyimide-poly perfluoroethylene propylene composite film has good stability, mechanical property and corona resistance, and the poly perfluoroethylene propylene layer and the polyimide film layer are stably attached and are not easy to separate.
2. The spherical alumina and boron nitride with a better proportion are used as the filling materials, the silane coupling agent KH792 is used as the modifier in the ethanol aqueous solution, sodium isostyrenesulfonate is used as the modification auxiliary agent, and the boron nitride is modified, so that the prepared filling materials have better dispersion uniformity, can be stably dispersed into the perfluoroethylene propylene dispersion liquid, further the perfluoroethylene propylene layer with uniform performance is prepared, and further the mechanical property, stability and corona resistance of the prepared corona-resistant polyimide-perfluoroethylene propylene composite film are improved.
3. The glycidyl methacrylate and the fluorocarbon surfactant with a better proportion are used as the leveling agent, so that the coating uniformity and stability of the prepared poly-perfluoroethylene propylene composite liquid on the surface of the polyimide film layer can be better improved, and further the corona-resistant polyimide-poly-perfluoroethylene propylene composite film with the poly-perfluoroethylene propylene layer and the polyimide film layer not being easily separated is prepared.
4. According to the preparation method, the prepared poly (perfluoroethylene-propylene) composite liquid is coated on the surface of the polyimide film layer, and then is subjected to sectional drying at a better temperature, so that the poly (perfluoroethylene-propylene) composite liquid forms a compact and stable poly (perfluoroethylene-propylene) layer, and is stably attached to the surface of the polyimide film layer, and the prepared corona-resistant polyimide-poly (perfluoroethylene-propylene) composite film has better corona resistance stability, and is not easy to separate from the polyimide film layer.
Detailed Description
The present application is described in further detail below with reference to examples.
The following are sources and specifications of some of the raw materials used in the present application, which are commercially available in the examples and preparations of the present application:
1. a dispersion of a perfluoroethylene propylene: the east Yue Shenzhou brand, DS603A/B, pH=7-9, surfactant content 3.5-8.0, solid content 48-55%;
2. spherical alumina: particle size is 100-200nm;
3. boron nitride: particle size 50-150nm;
4. maleic anhydride-acrylamide copolymer: commercially available, with a solids content of 30-40%, a ph=4-5, and an average molecular weight of 500-1000;
5. polyimide film: commercial, anpai, short-term heat-resistant temperature 320 ℃ and long-term heat-resistant temperature 200 ℃;
6. fluorocarbon surfactant: 3M,Fluorad FC 4430.
Preparation example of modified boron nitride
Preparation example 1
Preparation example 1 discloses a modified boron nitride, which is prepared by the following steps:
adding 5kg of boron nitride into 8kg of 50wt% ethanol water solution, uniformly stirring, heating to 60 ℃, adding 0.1kg of sodium isobenzenesulfonate and 0.2kg of silane coupling agent KH-792 for reaction for 1h, cooling, carrying out suction filtration, drying at 100 ℃, crushing and grinding to an average particle size of 50nm, and obtaining modified boron nitride for later use.
Preparation examples 2-3 disclose a modified boron nitride, which differs from preparation example 1 in the amount of raw materials and the preparation conditions, see in particular table 1 below.
TABLE 1 raw materials amounts and preparation conditions of preparation examples 1 to 3
Preparation example of polyperfluoroethylene propylene composite liquid
Preparation example 4
Preparation example 4 discloses a polyperfluoroethylene propylene composite solution, which is prepared by the following steps: 30kg of a perfluoroethylene propylene dispersion, a leveling agent consisting of 0.14kg of glycidyl methacrylate and 1.36kg of a fluorocarbon surfactant, 2.5kg of a maleic anhydride-acrylamide copolymer and a filler consisting of 2kg of spherical alumina and 2kg of commercially available boron nitride were added to a reaction kettle, and stirred for 1 hour at a stirring rate of 800rpm, and uniformly stirred to obtain a perfluoroethylene propylene composite solution.
Preparation examples 5 to 7
Preparation examples 5-7 disclose a polyperfluoroethylene propylene complex liquid, which is different from preparation example 4 in sources, amounts and preparation conditions of raw materials, and see table 2 below.
TABLE 2 raw material sources, amounts and preparation conditions of preparation examples 4 to 7
Preparation example 8
Preparation example 8 discloses a polyperfluoroethylene propylene composite liquid, which is different from preparation example 5 in the proportion of filler, the dosage of spherical alumina is 2.86kg, the dosage of boron nitride is 1.14kg, and the other materials are the same as preparation example 5.
Preparation example 9
Preparation example 9 discloses a polyperfluoroethylene propylene complex liquid, which is different from preparation example 5 in the proportion of filler, the amount of spherical alumina is 2.5kg, the amount of boron nitride is 1.5kg, and the other materials are the same as preparation example 5.
Preparation example 10
Preparation example 10 discloses a polyperfluoroethylene propylene complex liquid, which is different from preparation example 8 in the proportion of a leveling agent, the amount of glycidyl methacrylate is 0.35kg, the amount of fluorocarbon surfactant is 1.15kg, and the other is the same as preparation example 8.
PREPARATION EXAMPLE 11
Preparation 11 discloses a polyperfluoroethylene propylene complex liquid, which is different from preparation 8 in the proportion of a leveling agent, the amount of glycidyl methacrylate is 0.5kg, the amount of fluorocarbon surfactant is 1kg, and the other is the same as preparation 8.
Preparation example 12
Preparation example 12 discloses a polyperfluoroethylene propylene complex liquid, which is different from preparation example 5 in that glycidyl methacrylate is replaced by fluorocarbon surfactant in the same amount, and the other steps are the same as in preparation example 5.
Preparation example 13
Preparation example 13 discloses a polyperfluoroethylene propylene compound liquid, which is different from preparation example 5 in that the leveling agent is replaced by an organosilicon surfactant in an equivalent amount, and the other components are the same as preparation example 5.
PREPARATION EXAMPLE 14
Preparation example 14 discloses a polyperfluoroethylene propylene complex solution, which is different from preparation example 5 in that only one drying is performed, the drying temperature is 310 ℃, the drying time is 8min, and the other steps are the same as those of preparation example 5.
Preparation of comparative example 1
Preparation example comparative example discloses a polyperfluoroethylene propylene complex liquid, which is different from preparation example 5 in that the leveling agent is replaced by the polyperfluoroethylene propylene dispersion liquid in equal amount, and the other is the same as preparation example 5.
Preparation of comparative example 2
Preparation comparative example 2 discloses a polyperfluoroethylene propylene complex solution, which is different from preparation example 5 in that the maleic anhydride-acrylamide copolymer is replaced with a polyperfluoroethylene propylene dispersion solution in equal amount, and the other is the same as preparation example 5.
Examples
Example 1
Example 1 discloses a corona resistant polyimide-poly perfluoroethylene propylene composite film, which is prepared by the following steps:
the polyperfluoroethylene propylene complex liquid prepared in preparation example 5 was mixed at a concentration of 45g/m 2 Coating amount of (2) and coating speed of 2.5m/minAnd (3) coating the film on the surface of a polyimide film layer with the thickness of 75 mu m to form a poly (perfluoroethylene-propylene) layer, and then drying twice, wherein the first time is dried for 6min at the temperature of 260 ℃ and the second time is dried for 1min at the temperature of 310 ℃ to obtain the corona-resistant polyimide-poly (perfluoroethylene-propylene) composite film.
Examples 2 to 3
Examples 2-3 disclose a corona resistant polyimide-poly perfluoroethylene propylene composite film differing from example 1 in the source of the poly perfluoroethylene propylene composite solution and in the conditions for preparing the corona resistant polyimide-poly perfluoroethylene propylene composite film, see in particular table 3 below.
TABLE 3 Source of the polyperfluoroethylene propylene composite solutions of examples 1-3 and preparation condition Table of Corona-resistant polyimide-polyperfluoroethylene propylene composite film
Examples 4 to 11
Examples 4-11 disclose a corona resistant polyimide-poly perfluoroethylene propylene composite film differing from example 1 in the source of the poly perfluoroethylene propylene composite solution, as specifically set forth in Table 4 below.
TABLE 4 Source list of the polyperfluoroethylene propylene Complex solutions of examples 4-11
| Examples | Source of polyperfluoroethylene propylene composite liquid |
| Example 4 | Preparation example 4 |
| Example 5 | Preparation example 8 |
| Example 6 | Preparation example 9 |
| Example 7 | Preparation example 10 |
| Example 8 | PREPARATION EXAMPLE 11 |
| Example 9 | Preparation example 12 |
| Example 10 | Preparation example 13 |
| Example 11 | PREPARATION EXAMPLE 14 |
Comparative example
Comparative examples 1 to 2
Comparative examples 1-2 disclose a corona resistant polyimide-poiyperfluoroethylene propylene composite film differing from example 1 in the source of the poiyperfluoroethylene propylene composite solution, as specifically set forth in table 4 below.
TABLE 5 Source list of the polyperfluoroethylene propylene Complex solutions of comparative examples 1-2
| Comparative example | Source of polyperfluoroethylene propylene composite liquid |
| Comparative example 1 | Preparation of comparative example 1 |
| Comparative example 2 | Preparation of comparative example 2 |
Performance test the corona resistant polyimide-polyperfluoroethylene propylene composite films prepared in examples 1-11 and comparative examples 1-2 were subjected to performance test as follows:
(1) Tensile Strength test
Detecting and recording the detection result by referring to a test method in GB/T13542.2-2021 test method of electric insulation film part 2;
(2) Peel strength test
Detecting and recording the detection result by referring to the test method in ASTM-D3330, peel Strength test method;
(3) Corona resistance test
Referring to GB/T22689-2008 test method for measuring relative surface discharge breakdown resistance of solid insulating material, wherein the test voltage is 2kV, the test frequency is 20kHz, the pulse rise time is 50ns, the bipolar pulse square wave is a 6mm cylindrical electrode, the time of high-frequency pulse voltage resistance is tested, and the detection result is detected and recorded;
the following are performance test data for examples 1-11 and comparative examples 1-2, see in particular Table 5 below.
TABLE 5 Performance test data Table for examples 1-11 and comparative examples 1-2
As can be seen from the combination of examples 1-6 and table 5, the corona resistant polyimide-polyperfluoroethylene propylene composite film prepared by adding the spherical alumina and the modified boron nitride with the preferred proportions of the present application as fillers into the polyperfluoroethylene propylene composite liquid has improved tensile strength, peeling strength and corona resistant performance, and the corona resistant polyimide-polyperfluoroethylene propylene composite film prepared by compounding the commercial boron nitride with the spherical alumina has reduced performance in example 4 because the dispersion and the combination of the unmodified fillers and the system of the composite liquid are lower, so that the composite stability of the polyperfluoroethylene propylene layer formed by the polyperfluoroethylene propylene composite liquid and the polyimide film layer is lower.
It can be seen from the combination of examples 1 to 3 and examples 7 to 10, and comparative example 1 and table 5 that the corona resistant polyimide-polyperfluoroethylene propylene composite film prepared by using the glycidyl methacrylate and fluorocarbon surfactant in the preferred ratio of the present application as the leveling agent has improved tensile strength, improved peel strength and improved corona resistant performance, the fluorocarbon surfactant alone is used in example 9, the silicone surfactant is used as the leveling agent in example 10, and no leveling agent is added in comparative example 1, so that the performance of the corona resistant polyimide-polyperfluoroethylene propylene composite film prepared is reduced.
It can be seen from the combination of examples 1 to 3 and comparative example 2 and the combination of table 5 that by adding the maleic anhydride-acrylamide copolymer into the poly (perfluoroethylene-propylene) composite solution, the tensile strength, the peel strength and the corona resistance of the prepared corona-resistant polyimide-poly (perfluoroethylene-propylene) composite film can be better improved, because the maleic anhydride-acrylamide copolymer has better compatibility, the uniform mixing stability of the poly (perfluoroethylene-propylene) composite solution can be improved, and the adhesiveness of the formed poly (perfluoroethylene-propylene) layer and the polyimide film layer can be improved.
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 (9)
1. A corona resistant polyimide-poly perfluoroethylene propylene composite film is characterized in that,
the polyimide film comprises a polyimide film layer and a poly (perfluoroethylene propylene) layer arranged on the surface of the polyimide film layer, wherein the poly (perfluoroethylene propylene) layer is prepared by solidifying a poly (perfluoroethylene propylene) composite liquid, and the poly (perfluoroethylene propylene) composite liquid is prepared from the following raw materials in parts by weight:
60-80 parts of a dispersion of perfluoroethylene propylene
8-20 parts of filling material
3-8 parts of leveling agent
5-15 parts of maleic anhydride-acrylamide copolymer;
the leveling agent consists of glycidyl methacrylate and fluorocarbon surfactant in the dosage ratio of (0.3-0.5): 1.
2. The corona resistant polyimide-poly (perfluoroethylene propylene) composite film according to claim 1, wherein the filler consists of spherical aluminum oxide and boron nitride with the dosage ratio of 1 (0.4-0.6).
3. The corona resistant polyimide-poly perfluoroethylene propylene composite film according to claim 2, wherein the boron nitride is modified boron nitride, and the modified boron nitride is prepared from the following raw materials in parts by weight:
silane coupling agent KH-792-5 parts
1-3 parts of sodium isobenzenesulfonate
80-120 parts of 50-80wt% ethanol water solution
50-70 parts of boron nitride.
4. The corona resistant polyimide-poly perfluoroethylene propylene composite film according to claim 3, wherein said modified boron nitride is prepared by the steps of:
adding boron nitride into 50-80wt% ethanol water solution, stirring uniformly, heating to 60-70 ℃, adding sodium isobenzenesulfonate and silane coupling agent KH-792 for reaction for 1-2h, cooling, suction filtering, drying, crushing and grinding to obtain modified boron nitride.
5. The corona resistant polyimide-polyperfluoroethylene propylene composite film according to any one of claims 1-4, wherein said polyperfluoroethylene propylene composite solution is prepared by the steps of: adding the perfluoroethylene propylene dispersion liquid, the flatting agent, the maleic anhydride-acrylamide copolymer and the filler into stirring equipment, and uniformly stirring to obtain the perfluoroethylene propylene composite liquid.
6. The corona resistant polyimide-poly perfluoroethylene propylene composite film according to claim 5, wherein the mixing and stirring time is 1-3 hours and the stirring speed is 800-1200rpm.
7. The corona resistant polyimide-poly perfluoroethylene propylene composite film according to claim 1, wherein the poly perfluoroethylene propylene layer has a thickness of 20-50 μm.
8. A method for preparing a corona resistant polyimide-poly perfluoroethylene propylene composite film according to any one of claims 1 to 7, comprising the steps of:
and coating the poly (perfluoroethylene-propylene) composite liquid on the surface of the polyimide film layer to form a poly (perfluoroethylene-propylene) layer, and drying to obtain the corona-resistant polyimide-poly (perfluoroethylene-propylene) composite film.
9. The method for preparing the corona resistant polyimide-poly (perfluoroethylene-propylene) composite film according to claim 8, wherein the coating rate of the poly (perfluoroethylene-propylene) composite liquid is 1.5-2.5m/min, the drying is divided into two stages, the drying temperature of the first stage is 260-280 ℃, the drying time is 6-8min, the drying temperature of the second stage is 310-330 ℃ and the drying time is 1-3min.
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