WO2024082973A1 - Matériau composite de fibre de mica/aramide résistant à l'effet corona pour véhicules à nouvelle source d'énergie et son procédé de préparation - Google Patents
Matériau composite de fibre de mica/aramide résistant à l'effet corona pour véhicules à nouvelle source d'énergie et son procédé de préparation Download PDFInfo
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- WO2024082973A1 WO2024082973A1 PCT/CN2023/123390 CN2023123390W WO2024082973A1 WO 2024082973 A1 WO2024082973 A1 WO 2024082973A1 CN 2023123390 W CN2023123390 W CN 2023123390W WO 2024082973 A1 WO2024082973 A1 WO 2024082973A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- mica
- modified
- aramid fiber
- paper
- mica powder
- Prior art date
Links
- 239000010445 mica Substances 0.000 title claims abstract description 349
- 229910052618 mica group Inorganic materials 0.000 title claims abstract description 349
- 229920006231 aramid fiber Polymers 0.000 title claims abstract description 174
- 239000002131 composite material Substances 0.000 title claims abstract description 106
- 238000002360 preparation method Methods 0.000 title claims abstract description 31
- 239000000843 powder Substances 0.000 claims abstract description 209
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims abstract description 74
- 239000000853 adhesive Substances 0.000 claims abstract description 67
- 230000001070 adhesive effect Effects 0.000 claims abstract description 67
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 50
- 239000002245 particle Substances 0.000 claims abstract description 50
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 39
- 239000000463 material Substances 0.000 claims abstract description 37
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000002994 raw material Substances 0.000 claims abstract description 28
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000002657 fibrous material Substances 0.000 claims abstract description 24
- 239000003999 initiator Substances 0.000 claims abstract description 23
- 239000004760 aramid Substances 0.000 claims description 82
- 229920003235 aromatic polyamide Polymers 0.000 claims description 82
- 239000000835 fiber Substances 0.000 claims description 82
- 239000002002 slurry Substances 0.000 claims description 44
- 238000007731 hot pressing Methods 0.000 claims description 29
- 238000009210 therapy by ultrasound Methods 0.000 claims description 26
- 229920001577 copolymer Polymers 0.000 claims description 25
- 238000001035 drying Methods 0.000 claims description 25
- 238000000034 method Methods 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- 239000000243 solution Substances 0.000 claims description 17
- 238000003756 stirring Methods 0.000 claims description 17
- 238000002156 mixing Methods 0.000 claims description 16
- 238000001914 filtration Methods 0.000 claims description 11
- 238000010030 laminating Methods 0.000 claims description 11
- 239000000203 mixture Substances 0.000 claims description 10
- 239000004342 Benzoyl peroxide Substances 0.000 claims description 9
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical group C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims description 9
- 235000019400 benzoyl peroxide Nutrition 0.000 claims description 9
- 229920001774 Perfluoroether Polymers 0.000 claims description 7
- 239000004696 Poly ether ether ketone Substances 0.000 claims description 7
- 239000011248 coating agent Substances 0.000 claims description 7
- 238000000576 coating method Methods 0.000 claims description 7
- 229920002530 polyetherether ketone Polymers 0.000 claims description 7
- 238000003825 pressing Methods 0.000 claims description 5
- 239000004697 Polyetherimide Substances 0.000 claims description 4
- 229920001601 polyetherimide Polymers 0.000 claims description 4
- 239000004812 Fluorinated ethylene propylene Substances 0.000 claims description 3
- HQQADJVZYDDRJT-UHFFFAOYSA-N ethene;prop-1-ene Chemical group C=C.CC=C HQQADJVZYDDRJT-UHFFFAOYSA-N 0.000 claims description 3
- 229920000840 ethylene tetrafluoroethylene copolymer Polymers 0.000 claims description 3
- 229920009441 perflouroethylene propylene Polymers 0.000 claims description 3
- 238000005098 hot rolling Methods 0.000 claims description 2
- 238000010292 electrical insulation Methods 0.000 abstract description 2
- 230000007774 longterm Effects 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 99
- 238000012360 testing method Methods 0.000 description 16
- 238000009413 insulation Methods 0.000 description 10
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 10
- 230000015556 catabolic process Effects 0.000 description 9
- OPUXVIDSMSFXIU-UHFFFAOYSA-N n-[2-fluoro-5-[[9-(2-morpholin-4-ylethoxy)-11-oxo-6h-benzo[c][1]benzoxepin-3-yl]amino]phenyl]benzamide Chemical compound C1=C(NC(=O)C=2C=CC=CC=2)C(F)=CC=C1NC(C=1)=CC=C(C(C2=C3)=O)C=1OCC2=CC=C3OCCN1CCOCC1 OPUXVIDSMSFXIU-UHFFFAOYSA-N 0.000 description 9
- 239000007822 coupling agent Substances 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 238000002474 experimental method Methods 0.000 description 6
- IUVCFHHAEHNCFT-INIZCTEOSA-N 2-[(1s)-1-[4-amino-3-(3-fluoro-4-propan-2-yloxyphenyl)pyrazolo[3,4-d]pyrimidin-1-yl]ethyl]-6-fluoro-3-(3-fluorophenyl)chromen-4-one Chemical compound C1=C(F)C(OC(C)C)=CC=C1C(C1=C(N)N=CN=C11)=NN1[C@@H](C)C1=C(C=2C=C(F)C=CC=2)C(=O)C2=CC(F)=CC=C2O1 IUVCFHHAEHNCFT-INIZCTEOSA-N 0.000 description 5
- 230000004048 modification Effects 0.000 description 5
- 238000012986 modification Methods 0.000 description 5
- 238000000465 moulding Methods 0.000 description 5
- 239000011148 porous material Substances 0.000 description 5
- 230000003247 decreasing effect Effects 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 239000000178 monomer Substances 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 3
- 239000011268 mixed slurry Substances 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 239000004814 polyurethane Substances 0.000 description 3
- 229920002635 polyurethane Polymers 0.000 description 3
- 239000004593 Epoxy Substances 0.000 description 2
- 229920000784 Nomex Polymers 0.000 description 2
- 238000009825 accumulation Methods 0.000 description 2
- 229920003180 amino resin Polymers 0.000 description 2
- 230000004888 barrier function Effects 0.000 description 2
- 239000011449 brick Substances 0.000 description 2
- 238000006482 condensation reaction Methods 0.000 description 2
- 230000008878 coupling Effects 0.000 description 2
- 238000010168 coupling process Methods 0.000 description 2
- 238000005859 coupling reaction Methods 0.000 description 2
- 230000032798 delamination Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000010894 electron beam technology Methods 0.000 description 2
- 239000010419 fine particle Substances 0.000 description 2
- 239000012634 fragment Substances 0.000 description 2
- 230000000977 initiatory effect Effects 0.000 description 2
- 238000003780 insertion Methods 0.000 description 2
- 230000037431 insertion Effects 0.000 description 2
- 239000012774 insulation material Substances 0.000 description 2
- 230000016507 interphase Effects 0.000 description 2
- 230000001788 irregular Effects 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 2
- 239000004763 nomex Substances 0.000 description 2
- 229920000058 polyacrylate Polymers 0.000 description 2
- 229920001721 polyimide Polymers 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- 101001121408 Homo sapiens L-amino-acid oxidase Proteins 0.000 description 1
- 102100026388 L-amino-acid oxidase Human genes 0.000 description 1
- 239000004677 Nylon Substances 0.000 description 1
- 101100012902 Saccharomyces cerevisiae (strain ATCC 204508 / S288c) FIG2 gene Proteins 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 206010061592 cardiac fibrillation Diseases 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000001066 destructive effect Effects 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000002600 fibrillogenic effect Effects 0.000 description 1
- 239000010408 film Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- HCDGVLDPFQMKDK-UHFFFAOYSA-N hexafluoropropylene Chemical group FC(F)=C(F)C(F)(F)F HCDGVLDPFQMKDK-UHFFFAOYSA-N 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 150000004702 methyl esters Chemical class 0.000 description 1
- 229920001778 nylon Polymers 0.000 description 1
- 229920000364 para-Aramid fibril Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- 238000001238 wet grinding Methods 0.000 description 1
Classifications
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H11/00—Pulp or paper, comprising cellulose or lignocellulose fibres of natural origin only
- D21H11/14—Secondary fibres
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/01—Waste products, e.g. sludge
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/03—Non-macromolecular organic compounds
- D21H17/04—Hydrocarbons
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/03—Non-macromolecular organic compounds
- D21H17/05—Non-macromolecular organic compounds containing elements other than carbon and hydrogen only
- D21H17/06—Alcohols; Phenols; Ethers; Aldehydes; Ketones; Acetals; Ketals
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/03—Non-macromolecular organic compounds
- D21H17/05—Non-macromolecular organic compounds containing elements other than carbon and hydrogen only
- D21H17/14—Carboxylic acids; Derivatives thereof
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/20—Macromolecular organic compounds
- D21H17/33—Synthetic macromolecular compounds
- D21H17/34—Synthetic macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D21H17/36—Polyalkenyalcohols; Polyalkenylethers; Polyalkenylesters
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/20—Macromolecular organic compounds
- D21H17/33—Synthetic macromolecular compounds
- D21H17/34—Synthetic macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D21H17/37—Polymers of unsaturated acids or derivatives thereof, e.g. polyacrylates
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/63—Inorganic compounds
- D21H17/66—Salts, e.g. alums
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/63—Inorganic compounds
- D21H17/67—Water-insoluble compounds, e.g. fillers, pigments
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/63—Inorganic compounds
- D21H17/67—Water-insoluble compounds, e.g. fillers, pigments
- D21H17/68—Water-insoluble compounds, e.g. fillers, pigments siliceous, e.g. clays
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/63—Inorganic compounds
- D21H17/67—Water-insoluble compounds, e.g. fillers, pigments
- D21H17/69—Water-insoluble compounds, e.g. fillers, pigments modified, e.g. by association with other compositions prior to incorporation in the pulp or paper
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H21/00—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties
- D21H21/14—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties characterised by function or properties in or on the paper
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H27/00—Special paper not otherwise provided for, e.g. made by multi-step processes
Definitions
- the present application relates to the field of insulating materials, especially the technical field of mica composite materials, and more specifically to a corona-resistant mica/aramid fiber composite material for new energy vehicles and a preparation method thereof.
- Aramid fiber pure paper or NHN composite paper has high heat resistance and excellent performance in the insulation structure of 400V voltage platform motors for new energy vehicles.
- the maximum safe voltage may reach 2300V or even higher, which is far higher than the partial discharge inception voltage (PDIV) of existing conventional low-voltage motor insulation materials.
- PDIV partial discharge inception voltage
- the probability of partial discharge during motor operation is very high. Therefore, for 800V voltage platform automotive motors, the corona resistance of the insulation material must be considered.
- the existing technology improves the corona resistance life of composite paper by adding mica components to organic aramid fiber paper, or by using epoxy, polyurethane or polyacrylate adhesives to composite aramid fiber paper and mica paper.
- the mica-containing composite paper prepared by these two methods generally has problems such as easy powder loss, easy cracking, and delamination.
- the corona resistance and high temperature resistance are average, and cannot meet the process requirements for large-scale application of new energy vehicle motors.
- a corona-resistant mica/aramid fiber composite material for new energy vehicles and a preparation method thereof are provided.
- the present application provides modified mica materials and modified aramid fiber materials with excellent corona resistance, and uses PFA-tetrafluoroethylene-perfluoroalkoxy vinyl ether copolymer, FEP-fluorinated ethylene propylene copolymer (F46, tetrafluoroethylene and hexafluoropropylene copolymer), ETFE-ethylene-tetrafluoroethylene copolymer, PEEK-polyetheretherketone, PEI-polyetherimide and other high temperature resistant, low dielectric constant adhesives, and hot-presses the modified aramid fiber material and the modified mica material for compounding or mixing, which can improve the overall density and paper insertion processability, corona resistance, partial discharge inception voltage (PDIV) and temperature resistance grade of the composite material.
- PDIV partial discharge inception voltage
- a corona-resistant mica/aramid fiber composite material for new energy vehicles wherein the raw materials for preparing the composite material include: a modified aramid fiber material, an adhesive and a modified mica material;
- the adhesive comprises one or more of tetrafluoroethylene-perfluoroalkoxy vinyl ether copolymer, fluorinated ethylene propylene copolymer, ethylene-tetrafluoroethylene copolymer, polyetheretherketone and polyetherimide,
- the modified mica material is prepared from the following raw materials: mica powder, hydrochloric acid solution, ethanol, silane coupling agent, methyl methacrylate, initiator and toluene;
- the mica powder consists of a first mica powder, a second mica powder and a third mica powder, the particle size of the first mica powder is 90-110 ⁇ m, the particle size of the second mica powder is 130-150 ⁇ m, and the particle size of the third mica powder is 200-230 ⁇ m; the weight ratio of the first mica powder, the second mica powder and the third mica powder is 1:(3-5):(3-5) respectively.
- the adhesive is FEP-fluorinated ethylene propylene copolymer (F46, tetrafluoroethylene and hexafluoropropylene copolymer); further, the adhesive includes FEP-fluorinated ethylene propylene copolymer (F46, tetrafluoroethylene and hexafluoropropylene copolymer) and polyetheretherketone, with a weight ratio of 3:1.
- the concentration of the hydrochloric acid solution is 2 mol/L.
- the weight ratio of the silane coupling agent to the mica powder is (0.05-0.08):1, the weight ratio of the mica powder to methyl methacrylate and the initiator is 1:(0.1-0.15):(0.002-0.005) respectively, and the weight ratio of the mica powder to ethanol and toluene is 1:(6-8):(5-8) respectively.
- the method for preparing the modified mica material comprises the following steps:
- the mass concentration of the slurry is 3-5%.
- the silane coupling agent is A171, and the initiator is benzoyl peroxide.
- the modified aramid fiber material is prepared from meta-aramid chopped fibers and meta-aramid fibrids, the lengths of the meta-aramid chopped fibers and the meta-aramid fibrids are both 2-3 mm, and the weight ratio of the meta-aramid chopped fibers to the meta-aramid fibrids is 1:(2-2.5).
- the method for preparing the modified aramid fiber material comprises the following steps:
- the mass concentration of the slurry is 0.1-0.5%.
- the ultrasonic treatment step is 10 seconds per ultrasonic treatment, with an interval of 3 seconds, and a total ultrasonic treatment of 6-9 minutes; ultrasonic parameters: frequency is 10-20kHz, power is 500W.
- the modified aramid fiber material is modified aramid paper
- the modified mica material is modified mica paper.
- the weight percentages of the raw materials are: 40-60% of modified aramid fiber paper, 5-20% of adhesive and 40-60% of modified mica paper.
- the method for preparing the modified mica material further comprises: S14, adding water and stirring evenly to form a slurry, and then passing the slurry through a paper sheet forming machine to obtain the modified mica paper.
- the method for preparing the modified aramid fiber material further comprises: S23, papermaking the modified aramid fiber paper through a paper sheet forming machine.
- water is added during the process of "S21, dispersing the meta-aramid chopped fibers and the meta-aramid fibrids to form a slurry.
- the modified aramid fiber material is modified aramid fiber
- the modified mica material is modified mica powder.
- the weight ratio of the modified aramid fiber to the modified mica powder is (0.1-0.5):1, and the added amount of the adhesive is 5-10% of the total weight of the modified aramid fiber and the modified mica powder.
- a method for preparing the above-mentioned corona-resistant mica/aramid fiber composite material for new energy vehicles comprising the following steps:
- a method for preparing the above-mentioned corona-resistant mica/aramid fiber composite material for new energy vehicles comprising the following steps:
- the drying temperature is 120° C.
- the hot pressing temperature is 265-310° C.
- the hot pressing pressure is 20 MPa.
- the corona-resistant mica/aramid fiber composite material for new energy vehicles of the present application by using PFA-tetrafluoroethylene-perfluoroalkoxy vinyl ether copolymer, FEP-fluorinated ethylene propylene copolymer (F46, tetrafluoroethylene and hexafluoropropylene copolymer), ETFE-copolymer of ethylene and tetrafluoroethylene, PEEK-polyetheretherketone, PEI-polyetherimide and other high-temperature resistant, low dielectric constant adhesives to compound modified aramid fiber materials and modified mica materials, combined with modified mica materials and modified aramid fiber materials with excellent corona resistance, the overall density and paper insertion processability, corona resistance, partial discharge inception voltage (PDIV) and temperature resistance grade of the composite material can be improved.
- PFA-tetrafluoroethylene-perfluoroalkoxy vinyl ether copolymer FEP-fluorinated ethylene propylene cop
- the mica powder is limited to be composed of three mica powders with different particle sizes, and their respective proportions are limited at the same time.
- the large-particle mica powder layer is complete in flaky form, which can play a better stress transfer role, avoid the paper from breaking due to concentrated force, and at the same time give the paper a certain stiffness.
- the small-particle mica with a relatively small proportion is filled between the large mica flakes, which can give the paper better strength properties, reduce the destructive effect on the fibers, and form a "brick and mud" structure, which can give the paper better strength properties.
- the lamellar structure of the two larger mica powders can act as "bricks" to provide more More attachment carriers, and the regular arrangement of two larger particle size mica powders also gives the paper better flatness. It has a larger diameter-to-thickness ratio, and the high insulation effect of the layer in the Z direction has a good blocking effect on the current, delaying the formation of the current channel, effectively delaying the spread of the arc, reducing the fiber carbonization damage, reducing the size and area of the breakdown point, and improving the corona resistance.
- a mica material is modified by using a silane coupling agent and a polymer monomer. There are hydroxyl groups on the surface of the mica powder. A silane coupling agent A171 is used to introduce double bonds on the powder surface. Then, the monomer and the initiator are added to the mica powder liquid for polymerization. The vinyl on the surface of the mica powder is copolymerized with the monomer to realize surface grafting of the polymer, thereby improving its dispersibility in the slurry and ultimately improving its interface bonding performance with the modified aramid fiber material.
- the grafting rate on the surface of mica powder is increased by limiting the ratio of silane coupling agent to mica powder; and the coverage rate of polymer is increased by limiting the ratio of mica powder to monomer and initiator.
- meta-aramid chopped fibers and meta-aramid fibrils are used, and their lengths and ratios are limited.
- the chopped fibers are rod-shaped structures, while the fibrils are light and thin films. Within this ratio range, the fibrils will adhere to the rod-shaped chopped fibers, which helps the chopped fibers to form a scaffold and become the backbone to which the fibrils depend. When subjected to external force, they can transfer stress.
- the network structure interwoven by the chopped fibers makes the composite material high in density, excellent in corona resistance, and long in service life.
- the surface fibrillation degree of the aramid fibers can be enhanced, the surface active groups and surface energy can be increased, thereby improving the dispersion performance of the aramid chopped fibers.
- the specific surface area and surface roughness of the aramid fibers can be improved, the interweaving force of the chopped fibers and the precipitated fibers can be increased, the aramid fibers can be made into fibrils, and the mechanical interlocking effect between the fiber interfaces can be enhanced, thereby improving the mechanical properties and high temperature resistance of the composite material.
- the hot pressing temperature is limited so that the chopped fibers and precipitated fibers are fully softened and bonded, and at the same time, the adhesive is fully penetrated into the pores of the modified aramid fiber paper and the modified mica paper to form an overall dense composite material, thereby improving the tensile strength of the composite material and improving electrical properties.
- the adhesive is melted and softened, and fully penetrates into the gaps between the chopped fibers and the precipitated fibers, bonding them into a dense whole, thereby improving the strength of the mixed paper, avoiding problems such as delamination and powdering, and the paper inserting processability and electrical properties are good.
- FIG1 is a schematic diagram of the structure of a corona-resistant mica/aramid fiber composite material for new energy vehicles according to an embodiment of the present application
- FIG2 is a schematic diagram of the structure of the corona-resistant mica/aramid fiber blended paper for new energy vehicles involved in an embodiment of the present application.
- 21 modified aramid fiber
- 22 adhesive
- 23 modified mica powder.
- reagents or raw materials used in the present invention can be purchased through conventional channels. Unless otherwise specified, the reagents or raw materials used in the present invention are used in a conventional manner in the art or in accordance with the product instructions. In addition, any method and material similar or equivalent to the described content can be applied to the method of the present invention. The preferred implementation methods and materials in this patent are for demonstration purposes only.
- Mica raw materials with different particle sizes were prepared by wet grinding in a ball mill, the ball-to-material ratio was controlled to be 4:1, the mass ratio of small and medium balls was 1:1, the speed was set to 300 rpm, and the mica particle size and particle size distribution were measured by a laser particle size analyzer to prepare three types of mica slurries with different particle sizes.
- the present application provides two types of mica/aramid fiber composite materials.
- the first composite material can be considered as composite paper with a multi-layer structure
- the second composite material can be considered as mixed paper without a multi-layer structure or with an indistinguishable layered structure.
- the mica/aramid fiber composite material comprises a modified aramid fiber material, an adhesive and a modified mica material.
- the modified aramid fiber material is modified aramid fiber paper
- the modified mica material is modified mica paper
- the modified aramid fiber material is modified aramid fiber
- the modified mica material is modified mica powder.
- the first mica/aramid fiber composite material according to the present application is introduced.
- Example A1 Composite material A1#
- Composite material A1# is prepared from the following raw materials in weight percentage: 40% modified aramid fiber paper, 5% adhesive and 40% modified mica paper, wherein the adhesive is FEP-fluorinated ethylene propylene copolymer (F46, tetrafluoroethylene and hexafluoropropylene copolymer).
- the adhesive is FEP-fluorinated ethylene propylene copolymer (F46, tetrafluoroethylene and hexafluoropropylene copolymer).
- the modified mica paper is prepared from the following raw materials: mica powder, hydrochloric acid solution, ethanol, silane coupling agent, methyl methacrylate, initiator and toluene.
- the mica powder is composed of the first mica powder, the second mica powder and the third mica powder.
- the particle size of the first mica powder is 90 ⁇ m
- the particle size of the second mica powder is 130 ⁇ m
- the particle size of the third mica powder is 200 ⁇ m
- the weight ratio of the first mica powder, the second mica powder and the third mica powder is 1:3:3.
- the weight ratio of the silane coupling agent to the mica powder is 0.05:1, the weight ratio of the mica powder to methyl methacrylate and the initiator is 1:0.1:0.002, and the weight ratio of the mica powder to ethanol and toluene is 1:6:5.
- the preparation method of modified mica paper comprises the following steps:
- silane coupling agent A171 to ethanol, and use hydrochloric acid solution to adjust the pH value to 4; then add mica powder, heat to 60°C and stir for 1 hour; filter, wash and dry, then add the mixture to toluene, and add methyl methacrylate and benzoyl peroxide at the same time, react at 70°C for 2 hours, filter and dry at 110°C for 0.5 hour; add water and stir evenly to form a slurry with a mass concentration of 3%, and pass it through a paper sheet forming machine to obtain modified mica paper.
- the modified aramid fiber paper is made of meta-aramid short-cut fibers and meta-aramid fibrids.
- the length of the meta-aramid short-cut fibers and meta-aramid fibrids is 2 mm.
- the weight ratio of nylon precipitated fibers is 1:2.
- the preparation method of modified aramid fiber paper comprises the following steps:
- the meta-aramid short-cut fibers and meta-aramid precipitated fibers are dispersed and water is added to prepare a slurry with a mass concentration of 0.1%; after ultrasonic treatment, the modified aramid fiber paper is made by a paper sheet forming machine, and the thickness of the aramid fiber paper is 0.05 mm; the ultrasonic treatment steps are 10 seconds each time, 3 seconds interval, and a total of 6 minutes of ultrasonic treatment; ultrasonic parameters: frequency is 10kHz, power is 500W.
- the preparation method of composite material A1# comprises the following steps:
- the dried composite material A is subjected to hot roller hot pressing to finally obtain a corona-resistant mica/aramid fiber composite material A1# for new energy vehicles with a thickness of 0.25 mm.
- the drying temperature is 120°C
- the hot pressing temperature is 270°C
- the hot pressing pressure is 20MPa.
- Example A2 Composite material A2#
- Composite material A2# is prepared from the following raw materials in weight percentage: 50% modified aramid fiber paper, 10% adhesive and 40% modified mica paper, wherein the adhesive is FEP-fluorinated ethylene propylene copolymer (F46, tetrafluoroethylene and hexafluoropropylene copolymer).
- the modified mica paper is prepared from the following raw materials: mica powder, hydrochloric acid solution, ethanol, silane coupling agent, methyl methacrylate, initiator and toluene;
- the mica powder is composed of a first mica powder, a second mica powder and a third mica powder, the particle size of the first mica powder is 110 ⁇ m, the particle size of the second mica powder is 150 ⁇ m, and the particle size of the third mica powder is 230 ⁇ m;
- the weight ratio of the first mica powder, the second mica powder and the third mica powder is 1:5:5 respectively;
- the weight ratio of the silane coupling agent to the mica powder is 0.08:1, and the weight ratio of the mica powder to the methyl methacrylate and the initiator is 1:0.15:0.005, the weight ratio of mica powder to ethanol and toluene is 1:8:8 respectively;
- the preparation method of modified mica paper comprises the following steps: adding silane coupling agent A171 to ethanol, adjusting the pH value to 4 with hydroch
- the modified aramid fiber paper is prepared from meta-aramid chopped fibers and meta-aramid fibrils, the lengths of the meta-aramid chopped fibers and the meta-aramid fibrils are both 3 mm, and the weight ratio of the meta-aramid chopped fibers to the meta-aramid fibrils is 1:2.5;
- the preparation method of the modified aramid fiber paper comprises the following steps: the meta-aramid chopped fibers and the meta-aramid fibrils are dispersed and water is added to form a slurry with a mass concentration of 0.3%, and the modified aramid fiber paper is obtained by ultrasonic treatment through a paper sheet forming machine, and the thickness of the aramid fiber paper is 0.05 mm; the ultrasonic treatment step is 10 seconds each time, with an interval of 3 seconds, and a total ultrasonic treatment of 9 minutes; ultrasonic parameters: frequency is 20kHz, power is 500W.
- the preparation method of composite material A2# comprises the following steps:
- the drying temperature is 120°C
- the hot pressing temperature is 265°C
- the hot pressing pressure is 20MPa.
- Example A3 Composite material A3#
- the composite material A3# is prepared from the following raw materials in weight percentage: 60% of modified aramid fiber paper, 20% of adhesive and 40% of modified mica paper, wherein the adhesive is PFA-tetrafluoroethylene-perfluoroalkoxy vinyl ether copolymer.
- the modified mica paper is prepared from the following raw materials: mica powder, hydrochloric acid solution, ethanol, silane coupling agent, methyl methacrylate, initiator and toluene;
- the mica powder is composed of a first mica powder, a second mica powder and a third mica powder, the particle size of the first mica powder is 100 ⁇ m, the particle size of the second mica powder is 140 ⁇ m, and the particle size of the third mica powder is 220 ⁇ m;
- the weight ratio of the first mica powder, the second mica powder and the third mica powder is 1:4:4 respectively;
- the weight ratio of the silane coupling agent to the mica powder is 0.06:1, and the mica powder
- the weight ratio of mica powder to methyl methacrylate and initiator is 1:0.12:0.003
- the weight ratio of mica powder to ethanol and toluene is 1:7:6.
- the preparation method of modified mica paper comprises the following steps: adding silane coupling agent A171 to ethanol, adjusting the pH value to 4 with hydrochloric acid solution, adding mica powder, heating to 70°C and stirring for 2h, filtering, washing and drying, adding the mixture to toluene, adding methyl methacrylate and benzoyl peroxide at the same time, reacting at 80°C for 3h, filtering and drying at 120°C After drying for 1 hour, water was added and stirred evenly to form a slurry with a mass concentration of 5%, and the slurry was processed by a paper sheet forming machine to obtain modified mica paper.
- the modified aramid fiber paper is prepared from meta-aramid chopped fibers and meta-aramid fibrils, the lengths of the meta-aramid chopped fibers and the meta-aramid fibrils are both 2 mm, and the weight ratio of the meta-aramid chopped fibers to the meta-aramid fibrils is 1:2.2;
- the preparation method of the modified aramid fiber paper comprises the following steps: the meta-aramid chopped fibers and the meta-aramid fibrils are dispersed and water is added to form a slurry with a mass concentration of 0.5%, and the modified aramid fiber paper is obtained by ultrasonic treatment through a paper sheet forming machine, and the thickness of the aramid fiber paper is 0.05 mm; the ultrasonic treatment step is 10 seconds each time, with an interval of 3 seconds, and a total ultrasonic treatment of 7 minutes; ultrasonic parameters: frequency is 15kHz, power is 500W.
- the preparation method of composite material A3# comprises the following steps:
- the drying temperature is 120°C
- the hot pressing temperature is 310°C
- the hot pressing pressure is 20MPa.
- Example A4 Composite material A4#
- Example A4 The difference between Example A4 and Example A1 is that the adhesive in Example A4 is a fluorinated ethylene propylene copolymer (F46, a copolymer of tetrafluoroethylene and hexafluoropropylene) and polyetheretherketone in a weight ratio of 3:1, which is the same as both.
- F46 fluorinated ethylene propylene copolymer
- polyetheretherketone in a weight ratio of 3:1
- Comparative Example A1 is methyl etherified amino resin, and the rest are the same.
- Comparative Example A2 The difference between Comparative Example A2 and Example A3 is that the aramid fiber in Comparative Example A2 is not modified, and the rest is the same.
- Comparative Example A3 The difference between Comparative Example A3 and Example A3 is that the mica powder in Comparative Example A3 has a particle size of 50 ⁇ m and 90 ⁇ m.
- the weight ratio of the two mica powders is 1:3, and the rest are the same.
- Comparative Example A4 The difference between Comparative Example A4 and Example A3 is that the weight ratios of the first mica powder, the second mica powder and the third mica powder in Comparative Example A4 are 1:1.5:1.2 respectively, and the rest are the same.
- Comparative Example A5 The difference between Comparative Example A5 and Example A3 is that the weight ratio of the silane coupling agent to the mica powder in Comparative Example A5 is 0.12:1, and the rest are the same.
- Comparative Example A6 The difference between Comparative Example A6 and Example A3 is that in Comparative Example A6, only silane coupling agent KH550 is used to modify the mica powder, and the rest are the same.
- Comparative Example A7 The difference between Comparative Example A7 and Example A3 is that the aramid fiber used in Comparative Example A7 is para-aramid fibrid, and the rest are the same.
- Comparative Example A8 The difference between Comparative Example A8 and Example A3 is that the lengths of the intermediate aramid chopped fibers and the meta-aramid fibrids in Comparative Example A8 are both 5 mm, and the rest are the same.
- Comparative Example A9 The difference between Comparative Example A9 and Example A3 is that the weight ratio of the meso-aramid chopped fibers to the para-aramid fibrids in Comparative Example A9 is 1:1, and the rest are the same.
- Comparative Example A10 The difference between Comparative Example A10 and Example A3 is that the hot pressing molding temperature in Comparative Example A10 is 360° C., and the rest are the same.
- Comparative Example A11 is pure meta-aramid fiber paper with a thickness of 0.25 mm.
- Comparative Example A12 is a composite material A (commercially available material name NHN) prepared by using polyurethane as an adhesive and laminating 0.05 mm thick meta-aramid fiber paper on both sides of a polyimide film, with a thickness of 0.25 mm.
- NHN commercially available material name
- Breakdown voltage The test was carried out in accordance with the national standard GB/T1408.1-2006. The sample thickness was 0.25 mm. A ⁇ 25 mm/ ⁇ 75 mm cylindrical electrode system was used. The test was repeated 5 times and the average value was taken.
- PDIV partial discharge initiation voltage
- the composite materials A1#-4# prepared by the raw materials and methods specified in this application have good electrical properties, long square wave corona resistance life, excellent high temperature resistance and excellent mechanical properties.
- the comparison composite material A1# used a commonly used adhesive on the market, and the final result was average electrical performance and average high temperature resistance; in the comparison composite material A2#, the aramid fiber was not modified, and the final result was average electrical performance. The reason for this was analyzed to be that the aramid fiber was relatively inert and had poor interface bonding with other matrix materials.
- mica with small particle size will produce more mica fragments, most of which act as "mud and sand" components when added to paper.
- the irregular arrangement leads to loose paper structure, increased thickness, damaged paper mixed structure, decreased mechanical properties of paper, and increased porosity of paper.
- the electron beam is more likely to cause breakdown of the paper due to the reduction of the high insulation barrier of large pieces of mica in the Z direction.
- the proportion of small and medium-sized mica powder in the composite material A4# exceeds the range specified in this application, and the final electrical performance is average.
- the reason is analyzed as follows: as the amount of mica with smaller particles increases, the integrity of the mica layer is destroyed, the size of the longitudinal structure increases, the number of fine particles increases and gradually accumulates, the arrangement of mica sheets also changes from flat to oblique, and the mechanical properties decrease; at the same time, due to the damage of the mica layer structure, the small-particle mica with a large proportion appears granular, and the accumulation of particles produces a large number of pores, which limits the insulating effect of mica.
- the paper is subjected to electrical breakdown, the current is less obstructed and the current channel is shorter, resulting in a decrease in the overall insulation performance of the paper.
- the ratio of silane coupling agent to mica powder in composite material A5# exceeds the range specified in this application, and the final electrical performance is average.
- the reason is analyzed as follows: excessive amount of coupling agent will reduce the coupling efficiency due to condensation reaction, the grafting rate is low, and the modification effect is poor. Small amount of coupling agent will result in less coupling agent grafted on the surface.
- the composite material A7# uses para-aramid fiber precipitation, which has good mechanical properties, but poor electrical properties.
- the gas performance is average. The reason is that the para-molecular structure has excellent mechanical properties, but its electrical properties are poorer than those of the meta-structure. At the same time, its precipitated fibers have poor coating properties on short-cut fibers.
- the fiber length used in the comparative composite material A8# exceeds the range specified in this application, and the final electrical performance is average.
- the reason is analyzed as follows: the lengthening of the fibers increases the probability of entanglement between the fibers, making them difficult to disperse, increasing the unevenness of the hot-pressed composite paper, and further affecting the overall strength of the paper.
- the ratio of precipitated fibers to chopped fibers used in the comparative composite material A9# is smaller than the range specified in the present application, and the final electrical performance is average. The reason for this is that the chopped fibers are interspersed in the paper structure, which easily leads to the formation of pores in the paper. The small ratio of precipitated fibers results in poor bonding with the chopped fibers, making it difficult to exert their electrical and thermal properties.
- the hot pressing molding temperature of the comparative composite material A10# was higher than the range specified in this application, and the final electrical performance was average. The reason was that the high temperature caused the raw materials to age and the bonding force between the aramid fiber and the precipitated fiber decreased.
- the comparative composite materials A11#-12# were common composite materials A on the market, with average high temperature resistance and short corona resistance life.
- Example B1 Mixed Paper 1#
- Mixed paper 1# is prepared from the following raw materials: modified aramid fiber, adhesive and modified mica powder; the weight ratio of modified aramid fiber to modified mica powder is 0.1:1, the added amount of adhesive is 5% of the total weight of modified aramid fiber and modified mica powder, and the adhesive is PFA-tetrafluoroethylene-perfluoroalkoxy vinyl ether copolymer.
- the modified mica powder is prepared from the following raw materials: mica powder, hydrochloric acid solution, ethanol, silane coupling agent, methyl methacrylate, initiator and toluene.
- the mica powder is composed of the first mica powder, the second mica powder and the third mica powder.
- the particle size of the first mica powder is 90 ⁇ m
- the particle size of the second mica powder is 130 ⁇ m
- the particle size of the third mica powder is 200 ⁇ m.
- the weight ratio of the first mica powder, the second mica powder and the third mica powder is 1:3:3.
- the weight ratio of the silane coupling agent to the mica powder is 0.05:1, the weight ratio of the mica powder to methyl methacrylate and the initiator is 1:0.1:0.002, and the weight ratio of the mica powder to ethanol and toluene is 1:6:5.
- the preparation method of modified mica powder comprises the following steps:
- the mixture was then added to toluene, and methyl methacrylate and benzoyl peroxide were added at the same time, and the mixture was reacted at 70°C for 2 hours. After filtering, the mixture was dried at 110°C for 0.5 hours to obtain the modified mica powder.
- the modified aramid fiber is prepared from meta-aramid chopped fibers and meta-aramid fibrils, the lengths of the meta-aramid chopped fibers and the meta-aramid fibrils are both 2 mm, and the weight ratio of the meta-aramid chopped fibers to the meta-aramid fibrils is 1:2.
- the preparation method of modified aramid fiber comprises the following steps:
- the meta-aramid short fibers and the meta-aramid fibrids are dispersed to form a slurry
- the modified aramid fiber was obtained by drying after ultrasonic treatment; the ultrasonic treatment steps were 10 seconds each time, 3 seconds interval, and a total of 6 minutes of ultrasonic treatment; the ultrasonic parameters were: frequency of 10 kHz and power of 500 W.
- the preparation method of mixed paper 1# comprises the following steps:
- the pressing time is 5 minutes
- the pressure is 300 kPa
- the hot pressing temperature is 310°C
- the hot pressing pressure is 20 MPa.
- Example B2 Mixed Paper 2#
- Mixed paper 2# is prepared from the following raw materials: modified aramid fiber, adhesive and modified mica powder; the weight ratio of modified aramid fiber to modified mica powder is 0.5:1, the added amount of adhesive is 10% of the total weight of modified aramid fiber and modified mica powder, and the adhesive is FEP-fluorinated ethylene propylene copolymer (F46, tetrafluoroethylene and hexafluoropropylene copolymer).
- the modified mica powder is prepared from the following raw materials: mica powder, hydrochloric acid solution, ethanol, silane coupling agent, methyl methacrylate, initiator and toluene;
- the mica powder is composed of a first mica powder, a second mica powder and a third mica powder, the particle size of the first mica powder is 110 ⁇ m, the particle size of the second mica powder is 150 ⁇ m, and the particle size of the third mica powder is 230 ⁇ m;
- the weight ratio of the first mica powder, the second mica powder and the third mica powder is 1:5:5 respectively;
- the weight ratio of the silane coupling agent to the mica powder is 0.08:1, and the mica powder
- the weight ratio of mica powder to methyl methacrylate and initiator is 1:0.15:0.005, and the weight ratio of mica powder to ethanol and toluene is 1:8:8.
- the preparation method of modified mica powder comprises the following steps: adding silane coupling agent A171 to ethanol, adjusting the pH value to 4 with hydrochloric acid solution, adding mica powder, heating to 80°C and stirring for 3h, filtering, washing and drying, adding the mixture to toluene, adding methyl methacrylate and benzoyl peroxide at the same time, reacting at 90°C for 4h, filtering and drying at 130°C
- the modified mica powder was obtained after drying for 2 hours.
- the modified aramid fiber is prepared from meta-aramid chopped fibers and meta-aramid fibrils, the lengths of the meta-aramid chopped fibers and the meta-aramid fibrils are both 3 mm, and the weight ratio of the meta-aramid chopped fibers to the meta-aramid fibrils is 1:2.5;
- the preparation method of the modified aramid fiber comprises the following steps: the meta-aramid chopped fibers and the meta-aramid fibrils are dispersed to form a slurry, and the slurry is dried after ultrasonic treatment to obtain the modified aramid fiber; the ultrasonic treatment step is 10 seconds each time, with an interval of 3 seconds, and a total ultrasonic treatment of 9 minutes; ultrasonic parameters: frequency is 20 kHz, and power is 500 W.
- the preparation method of mixed paper 2# comprises the following steps:
- the pressing time is 5 minutes
- the pressure is 300kPa
- the hot pressing temperature is 265°C
- the hot pressing pressure is 20MPa.
- Example B3 Mixed Paper 3#
- Mixed paper 3# is prepared from the following raw materials: modified aramid fiber, adhesive and modified mica powder; the weight ratio of modified aramid fiber to modified mica powder is 0.3:1, the added amount of adhesive is 8% of the total weight of modified aramid fiber and modified mica powder, and the adhesive is PFA-tetrafluoroethylene-perfluoroalkoxy vinyl ether copolymer.
- the modified mica powder is prepared from the following raw materials: mica powder, hydrochloric acid solution, ethanol, silane coupling agent, methyl methacrylate, initiator and toluene;
- the mica powder is composed of a first mica powder, a second mica powder and a third mica powder, the particle size of the first mica powder is 100 ⁇ m, the particle size of the second mica powder is 140 ⁇ m, and the particle size of the third mica powder is 220 ⁇ m;
- the weight ratio of the first mica powder, the second mica powder and the third mica powder is 1:4:4 respectively;
- the weight ratio of the silane coupling agent to the mica powder is 0.06:1, and the weight ratio of the mica powder to the methyl methacrylate is 0.06:1.
- the weight ratio of methyl ester and initiator is 1:0.12:0.003, and the weight ratio of mica powder to ethanol and toluene is 1:7:6.
- the preparation method of modified mica powder comprises the following steps: adding silane coupling agent A171 to ethanol, adjusting the pH value to 4 with hydrochloric acid solution, adding mica powder, heating to 70°C and stirring for 2h, filtering, washing and drying, adding the mixture to toluene, adding methyl methacrylate and benzoyl peroxide at the same time, reacting at 80°C for 3h, filtering and drying at 120°C for 1h to obtain modified mica powder.
- the modified aramid fiber is prepared from meta-aramid chopped fibers and meta-aramid fibrils, the lengths of the meta-aramid chopped fibers and the meta-aramid fibrils are both 2 mm, and the weight ratio of the meta-aramid chopped fibers to the meta-aramid fibrils is 1:2.2;
- the preparation method of the modified aramid fiber comprises the following steps: the meta-aramid chopped fibers and the meta-aramid fibrils are dispersed to form a slurry, and the slurry is dried after ultrasonic treatment to obtain the modified aramid fiber; the ultrasonic treatment step is 10 seconds each time, with an interval of 3 seconds, and a total ultrasonic treatment of 7 minutes; ultrasonic parameters: frequency is 15 kHz, and power is 500 W.
- the preparation method of mixed paper 3# comprises the following steps:
- the pressing time is 5 minutes
- the pressure is 300 kPa
- the hot pressing temperature is 302°C
- the hot pressing pressure is 20 MPa.
- Example B4 Mixed Paper 4#
- Example B4 The difference between Example B4 and Example B1 is that the adhesive in Example B4 is FEP-fluorinated ethylene propylene copolymer (F46, tetrafluoroethylene and hexafluoropropylene copolymer) and PEEK-polyetheretherketone, the weight ratio is 3:1, and the rest are the same.
- the adhesive in Example B4 is FEP-fluorinated ethylene propylene copolymer (F46, tetrafluoroethylene and hexafluoropropylene copolymer) and PEEK-polyetheretherketone, the weight ratio is 3:1, and the rest are the same.
- Comparative Example B1 is methyl etherified amino resin, and the rest are the same.
- Comparative Example B2 Comparative Mixed Paper 2#
- Comparative Example B2 The difference between Comparative Example B2 and Example B3 is that the aramid fiber in Comparative Example B2 is not modified, and the rest is the same.
- Comparative Example B3 The difference between Comparative Example B3 and Example B3 is that the weight ratio of the modified aramid fiber to the modified mica powder in Comparative Example B3 is 1.2:1, and the rest are the same.
- Comparative Example B4 The difference between Comparative Example B4 and Example B3 is that the mica powder in Comparative Example B4 has a particle size of 50 ⁇ m and 90 ⁇ m. The weight ratio of the two mica powders is 1:3, and the rest are the same.
- Comparative Example B5 Comparative Mixed Paper 5#
- Comparative Example B5 The difference between Comparative Example B5 and Example B3 is that the weight ratios of the first mica powder, the second mica powder and the third mica powder in Comparative Example B5 are 1:1.5:1.2 respectively, and the rest are the same.
- Comparative Example B6 The difference between Comparative Example B6 and Example B3 is that the weight ratio of the silane coupling agent to the mica powder in Comparative Example B6 is 0.12:1, and the rest are the same.
- Comparative Example B7 The difference between Comparative Example B7 and Example B3 is that in Comparative Example B7, only silane coupling agent KH550 is used to modify the mica powder, and the rest are the same.
- Comparative Example B8 is para-aramid fibrid, and the rest are the same.
- Comparative Example B9 The difference between Comparative Example B9 and Example B3 is that the lengths of the intermediate aramid chopped fibers and the meta-aramid fibrids in Comparative Example B9 are both 5 mm, and the rest are the same.
- Comparative Example B10 Comparative Mixed Paper 10#
- Comparative Example B10 The difference between Comparative Example B10 and Example B3 is that the weight ratio of the meso-aramid chopped fibers to the meta-aramid fibrids in Comparative Example B10 is 1:1, and the rest are the same.
- Comparative Example B11 The difference between Comparative Example B11 and Example B3 is that the hot pressing molding temperature in Comparative Example B11 is 380° C., and the rest are the same.
- Comparative Example B12 is commercially available meta-aramid fiber paper, pure paper, with a thickness of 0.25 mm.
- Breakdown voltage The test was carried out in accordance with the national standard GB/T1408.1 2006. The sample thickness was 0.25 mm. A ⁇ 25 mm/ ⁇ 75 mm cylindrical electrode system was used. The test was repeated 5 times and the average value was taken.
- PDIV Partial Discharge Initiation Voltage
- Composite materials B1#-4#, comparative composite materials B1#-11#, and meta-aramid fiber paper were sampled and tested for the above four tests. The experimental results are shown in Table 2.
- the mixed paper 1#-4# prepared by the raw materials and methods specified in this application has good electrical properties, long square wave corona resistance life, excellent high temperature resistance and excellent mechanical properties.
- the comparison mixed paper 1# used a commonly used adhesive on the market, and the final result was average electrical properties and average high temperature resistance; the comparison mixed paper 2# did not modify the aramid fiber, and the final result was average electrical properties.
- the reason was analyzed as the aramid fiber is relatively inert and has poor interface bonding with the matrix material.
- the ratio of modified aramid fiber to modified mica powder in mixed paper 3# exceeds the range specified in this application, and the final electrical performance is average.
- the reason is analyzed to be that the combination of aramid fiber and mica has been saturated, and excessive fibers accumulate in the gaps formed by mica scales or on the surface of the scales, causing the paper thickness to increase, resulting in uneven distribution of the electric field in the paper structure, generating a large amount of heat that cannot be dissipated, resulting in a decrease in the breakdown field strength.
- mica powder in mixed paper 4# is smaller than the range specified in this application, and the final electrical performance is average.
- the reason is analyzed as follows: mica with small particle size will produce more mica fragments, most of which act as "silt" components when added to paper.
- the irregular arrangement leads to a decrease in the fit between mica and fiber, a loose paper structure, increased thickness, damaged paper mixed structure, and a decrease in paper mechanical properties.
- the porosity of the paper increases.
- the electron beam is more likely to cause breakdown of the paper due to the reduction of the high insulation barrier of large pieces of mica in the Z direction.
- the proportion of small and medium-sized mica powder in mixed paper 5# exceeds the range specified in this application, and the final electrical performance is average.
- the reason is analyzed as follows: as the amount of mica with smaller particles increases, the integrity of the mica layer is destroyed, the size of the longitudinal structure increases, the number of fine particles increases and gradually accumulates, and the arrangement of mica sheets also changes from flat to oblique, resulting in poor bonding between fibers and mica and decreased mechanical properties; at the same time, due to the damage of the mica layer structure, the small-particle mica with a large proportion is granular, and the accumulation of particles produces a large number of pores, which limits the insulating effect of mica. When the paper is subjected to electrical breakdown, the current is less obstructed and the current channel is shorter, resulting in a decrease in the overall insulation performance of the paper.
- the ratio of silane coupling agent to mica powder in mixed paper 6# exceeds the range specified in this application, and the final electrical performance is average.
- the reason is that the excessive amount of coupling agent reduces the coupling efficiency due to condensation reaction, and the grafting rate is low.
- the modification effect is poor, and the smaller the amount of coupling agent used, the less coupling agent is grafted on the surface.
- para-aramid fibrils are used in mixed paper 8#, and the final result shows good mechanical properties, but average electrical properties.
- the reason is that the para-molecular structure shows excellent mechanical properties, but the electrical properties are poorer than those of the meta-structure.
- the fibrils have poor coating properties on short-cut fibers.
- the fiber length used in the mixed paper 9# exceeds the range specified in this application, and the final electrical performance is average.
- the reason is analyzed to be that the lengthening of the fibers increases the probability of entanglement between the fibers, making them difficult to disperse, increasing the unevenness of the hot-pressed composite paper, and thus affecting the overall strength of the paper.
- the ratio of precipitated fibers to chopped fibers used in mixed paper 10# is smaller than the range specified in the present application, and the final electrical performance is average.
- the reason is analyzed to be that the chopped fibers have no bonding force with mica.
- the chopped fibers have a relatively large thickness relative to mica, and are interspersed in the paper structure, which has a certain degree of damage to the bonding between precipitated fibers and mica, resulting in easy formation of pores in the paper.
- a small ratio of precipitated fibers will result in poor bonding between the chopped fibers and mica, making it difficult to exert their electrical and thermal properties.
- the hot pressing molding temperature of the mixed paper 11# was higher than the range specified in this application, and the final result had average electrical properties.
- the reason for this was that the high temperature caused the raw materials to age, and the bonding force between the aramid fiber, precipitated fiber and mica powder decreased.
- the meta-aramid fiber paper of comparative example B12 did not contain mica components, and the final result had average electrical properties and average high temperature resistance, but good mechanical properties.
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Abstract
L'invention concerne un matériau composite de fibre de mica/aramide résistant à l'effet corona pour véhicules à nouvelle source d'énergie et son procédé de préparation. Les matières premières de préparation comprennent un matériau de fibre d'aramide modifié, un adhésif et un matériau de mica modifié ; le matériau de mica modifié comprend de la poudre de mica, une solution d'acide chlorhydrique, de l'éthanol, un agent de couplage au silane, du méthacrylate de méthyle, un initiateur et du méthylbenzène ; la poudre de mica est composée d'une première poudre de mica, d'une deuxième poudre de mica et d'une troisième poudre de mica, la granulométrie de la première poudre de mica étant de 90 à 110 µm, la granulométrie de la deuxième poudre de mica étant de 130 à 150 µm, et la granulométrie de la troisième poudre de mica étant de 200 à 230 µm ; et le rapport en poids de la première poudre de mica à la deuxième poudre de mica à la troisième poudre de mica est de 1:(3-5):(3-5). Le matériau en fibre aramide modifiée et le matériau en mica modifié sont combinés à l'aide d'un adhésif, de sorte que la compacité globale, la fabricabilité du papier interpolé, la résistance à l'effet corona, la TADP et le seuil de résistance à la température du matériau composite sont améliorés, et le matériau peut considérablement améliorer la performance d'isolation électrique et la durée de vie sûre à long terme des véhicules à nouvelle source d'énergie.
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CN202211286451.7A CN115584660B (zh) | 2022-10-20 | 2022-10-20 | 一种新能源汽车用耐电晕云母/芳纶纤维混抄纸及其制备方法 |
CN202211286443.2 | 2022-10-20 | ||
CN202211286451.7 | 2022-10-20 | ||
CN202211286443.2A CN115538215B (zh) | 2022-10-20 | 2022-10-20 | 一种新能源汽车用耐电晕云母/芳纶纤维复合材料及其制备方法 |
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